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The triclinic structures of dicobalt and dinickel 4,4′-bi­phenyldi­carboxyl­ate di­hydroxide, M2(O2CC6H4C6H4CO2)(OH)2 were established using laboratory X-ray powder diffraction data. These structures, as well as that of Mn2(O2CC6H4C6H4CO2)(OH)2, were optimized using density functional techniques. The structure of di­ammonium 4,4′-bi­phenyldi­carboxyl­ate was also solved using laboratory powder data.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989022009288/hb8029sup1.cif
Contains datablocks Co_X, Ni_X, UBUPEQ_DFT, NH4_X, global, Co_DFT, Ni_DFT, NH4_DFT

CCDC references: 2208530; 2208529; 2208528; 2208527; 2208526; 2208525; 2208524

Key indicators

  • Powder X-ray study
  • T = 300 K
  • Mean [sigma](C-C) = 0.060 Å
  • Mean [sigma](C-C) = 0.164 Å
  • Mean [sigma](C-C) = 0.000 Å
  • Mean [sigma](C-C) = 0.034 Å
  • R factor = 0.000
  • wR factor = 0.104
  • Data-to-parameter ratio = 0.0

checkCIF/PLATON results

No syntax errors found



Datablock: Co_X


Alert level A PLAT080_ALERT_2_A Maximum Shift/Error ............................ 2.59 Why ? PLAT701_ALERT_1_A Bond Calc 16.07(6), Rep 2.105(9), Dev.. 232.75 Sigma O12 -CO14 1_555 1_656 ........ # 19 Check PLAT701_ALERT_1_A Bond Calc 5.42(2), Rep 2.098(8), Dev.. 166.10 Sigma O16 -CO14 1_555 1_555 ........ # 22 Check PLAT701_ALERT_1_A Bond Calc 7.24(3), Rep 2.121(8), Dev.. 170.63 Sigma O16 -CO14 1_555 1_556 ........ # 23 Check PLAT701_ALERT_1_A Bond Calc 16.07(6), Rep 2.105(9), Dev.. 232.75 Sigma CO14 -O12 1_555 1_454 ........ # 26 Check PLAT701_ALERT_1_A Bond Calc 12.09(4), Rep 2.105(9), Dev.. 249.63 Sigma CO14 -O12 1_555 2_656 ........ # 27 Check PLAT701_ALERT_1_A Bond Calc 7.24(3), Rep 2.121(8), Dev.. 170.63 Sigma CO14 -O16 1_555 1_554 ........ # 28 Check PLAT701_ALERT_1_A Bond Calc 5.42(2), Rep 2.098(8), Dev.. 166.10 Sigma CO14 -O16 1_555 1_555 ........ # 29 Check PLAT701_ALERT_1_A Bond Calc 27.92(10), Rep 2.098(8), Dev.. 258.22 Sigma CO14 -O16 1_555 2_555 ........ # 30 Check PLAT701_ALERT_1_A Bond Calc 28.04(10), Rep 2.121(8), Dev.. 259.19 Sigma CO14 -O16 1_555 2_556 ........ # 31 Check PLAT701_ALERT_1_A Bond Calc 27.85(10), Rep 2.028(8), Dev.. 258.22 Sigma CO15 -O16 1_555 2_566 ........ # 33 Check
Alert level B SYMMS02_ALERT_1_B No unit-cell angle should be equal to 90 for a triclinic cell Cell 14.1600 6.2685 3.3230 Angles 91.4270 98.4600 90.0000 PLAT149_ALERT_3_B s.u. on the gamma Angle is Too Large ....... 0.30 Degree PLAT241_ALERT_2_B High 'MainMol' Ueq as Compared to Neighbors of C5 Check PLAT242_ALERT_2_B Low 'MainMol' Ueq as Compared to Neighbors of C11 Check PLAT341_ALERT_3_B Low Bond Precision on C-C Bonds ............... 0.06 Ang.
Alert level C PLAT148_ALERT_3_C s.u. on the a - Axis is (Too) Large .... 0.050 Ang. PLAT148_ALERT_3_C s.u. on the c - Axis is (Too) Large .... 0.004 Ang. PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced .......... Please Do ! PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of Co15 Check PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C1 - H2 . 1.16 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C3 - H4 . 1.15 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C6 - H7 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C8 - H9 . 1.14 Ang. PLAT410_ALERT_2_C Short Intra H...H Contact H2 ..H9 . 1.96 Ang. 1-x,1-y,2-z = 2_667 Check PLAT751_ALERT_4_C Bond Calc 0.99000, Rep 0.992(13) ...... Senseless s.u. O16 -H17 1_555 1_555 ........ # 21 Check PLAT751_ALERT_4_C Bond Calc 0.99000, Rep 0.992(13) ...... Senseless s.u. H17 -O16 1_555 1_555 ........ # 25 Check PLAT762_ALERT_1_C CIF Contains no X-Y-H or H-Y-H Angles .......... Please Check
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C14 H10 Co2 O6 Atom count from _chemical_formula_moiety:C7 H5 Co1 O3 PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension 3 Info PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 1 Report PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... 2 Check PLAT092_ALERT_4_G Check: Wavelength Given is not Cu,Ga,Mo,Ag,In Ka 0.71361 Ang. PLAT152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ... 9 Units PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.41 Ratio PLAT769_ALERT_4_G CIF Embedded explicitly supplied scattering data Please Note PLAT794_ALERT_5_G Tentative Bond Valency for Co14 (II) . 1.95 Info PLAT794_ALERT_5_G Tentative Bond Valency for Co15 (II) . 1.90 Info PLAT804_ALERT_5_G Number of ARU-Code Packing Problem(s) in PLATON 4 Info PLAT984_ALERT_1_G The Co-f'= 0.3490 Deviates from the B&C-Value 0.3510 Check PLAT985_ALERT_1_G The Co-f"= 0.9720 Deviates from the B&C-Value 0.9844 Check
11 ALERT level A = Most likely a serious problem - resolve or explain 5 ALERT level B = A potentially serious problem, consider carefully 12 ALERT level C = Check. Ensure it is not caused by an omission or oversight 13 ALERT level G = General information/check it is not something unexpected 17 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 8 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion 5 ALERT type 5 Informative message, check
Datablock: Ni_X

Alert level A CELLV01_ALERT_1_A The supplied cell volume differs from that calculated from the cell parameters. Ratio outside the range 0.999 < > 1.001 Calculated cell volume = 344.139 Cell volume given = 345.300 PLAT080_ALERT_2_A Maximum Shift/Error ............................ 4.43 Why ? PLAT341_ALERT_3_A Low Bond Precision on C-C Bonds ............... 0.16375 Ang. PLAT701_ALERT_1_A Bond Calc 15.8(12), Rep 1.953(12), Dev.. 11.54 Sigma O13 -NI15 1_555 1_654 ........ # 21 Check PLAT701_ALERT_1_A Bond Calc 14.4(11), Rep 1.927(19), Dev.. 11.34 Sigma NI14 -O16 1_555 1_654 ........ # 24 Check PLAT701_ALERT_1_A Bond Calc 14.4(11), Rep 1.927(19), Dev.. 11.34 Sigma NI14 -O16 1_555 2_656 ........ # 25 Check PLAT701_ALERT_1_A Bond Calc 14.4(11), Rep 1.927(19), Dev.. 11.34 Sigma O16 -NI14 1_555 1_456 ........ # 26 Check PLAT701_ALERT_1_A Bond Calc 5.2(4), Rep 1.919(13), Dev.. 8.20 Sigma O16 -NI15 1_555 1_555 ........ # 27 Check PLAT701_ALERT_1_A Bond Calc 15.8(12), Rep 1.953(12), Dev.. 11.54 Sigma NI15 -O13 1_555 1_456 ........ # 28 Check PLAT701_ALERT_1_A Bond Calc 12.9(10), Rep 1.953(12), Dev.. 10.95 Sigma NI15 -O13 1_555 2_665 ........ # 29 Check PLAT701_ALERT_1_A Bond Calc 5.2(4), Rep 1.919(13), Dev.. 8.20 Sigma NI15 -O16 1_555 1_555 ........ # 30 Check PLAT701_ALERT_1_A Bond Calc 29(2), Rep 1.919(13), Dev.. 13.54 Sigma NI15 -O16 1_555 2_566 ........ # 31 Check
Alert level B PLAT149_ALERT_3_B s.u. on the alpha Angle is Too Large ....... 0.23 Degree PLAT149_ALERT_3_B s.u. on the beta Angle is Too Large ....... 0.80 Degree PLAT149_ALERT_3_B s.u. on the gamma Angle is Too Large ....... 2.30 Degree PLAT241_ALERT_2_B High 'MainMol' Ueq as Compared to Neighbors of O12 Check PLAT241_ALERT_2_B High 'MainMol' Ueq as Compared to Neighbors of O13 Check PLAT241_ALERT_2_B High 'MainMol' Ueq as Compared to Neighbors of C11 Check PLAT242_ALERT_2_B Low 'MainMol' Ueq as Compared to Neighbors of Ni14 Check PLAT242_ALERT_2_B Low 'MainMol' Ueq as Compared to Neighbors of C5 Check PLAT369_ALERT_2_B Long C(sp2)-C(sp2) Bond C5 - C11 . 1.64 Ang. PLAT410_ALERT_2_B Short Intra H...H Contact H2 ..H9 . 1.83 Ang. 1-x,1-y,-z = 2_665 Check
Alert level C PLAT148_ALERT_3_C s.u. on the a - Axis is (Too) Large .... 1.100 Ang. PLAT148_ALERT_3_C s.u. on the b - Axis is (Too) Large .... 0.120 Ang. PLAT148_ALERT_3_C s.u. on the c - Axis is (Too) Large .... 0.090 Ang. PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced .......... Please Do ! PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C1 - H2 . 1.13 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C3 - H4 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C6 - H7 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C8 - H9 . 1.14 Ang. PLAT761_ALERT_1_C CIF Contains no X-H Bonds ...................... Please Check PLAT762_ALERT_1_C CIF Contains no X-Y-H or H-Y-H Angles .......... Please Check
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C14 H10 Ni2 O6 Atom count from _chemical_formula_moiety:C7 H5 Ni1 O3 PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension 2 Info PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 1 Report PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... 2 Check PLAT092_ALERT_4_G Check: Wavelength Given is not Cu,Ga,Mo,Ag,In Ka 1.54445 Ang. PLAT152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ... 25 Units PLAT303_ALERT_2_G Full Occupancy Atom H17 with # Connections 3.00 Check PLAT335_ALERT_2_G Check Large C6 Ring C-C Range C1 -C10 0.21 Ang. PLAT432_ALERT_2_G Short Inter X...Y Contact C1 ..C6 . 2.40 Ang. x,y,-1+z = 1_554 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C1 ..C8 . 2.80 Ang. x,y,-1+z = 1_554 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C1 ..C5 . 3.10 Ang. x,y,-1+z = 1_554 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C3 ..C6 . 2.70 Ang. x,y,-1+z = 1_554 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C3 ..C5 . 3.00 Ang. x,y,-1+z = 1_554 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C3 ..C11 . 3.10 Ang. x,y,-1+z = 1_554 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C6 ..C10 . 2.90 Ang. x,y,1+z = 1_556 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C8 ..C8 . 2.90 Ang. 1-x,1-y,1-z = 2_666 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C8 ..C10 . 3.00 Ang. x,y,1+z = 1_556 Check PLAT432_ALERT_2_G Short Inter X...Y Contact C8 ..C10 . 3.00 Ang. 1-x,1-y,1-z = 2_666 Check PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.72 Ratio PLAT769_ALERT_4_G CIF Embedded explicitly supplied scattering data Please Note PLAT794_ALERT_5_G Tentative Bond Valency for Ni14 (II) . 1.90 Info PLAT794_ALERT_5_G Tentative Bond Valency for Ni15 (II) . 1.87 Info PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 30 Note PLAT984_ALERT_1_G The Ni-f'= -3.0020 Deviates from the B&C-Value -2.9351 Check PLAT985_ALERT_1_G The Ni-f"= 0.5090 Deviates from the B&C-Value 0.5123 Check
12 ALERT level A = Most likely a serious problem - resolve or explain 10 ALERT level B = A potentially serious problem, consider carefully 10 ALERT level C = Check. Ensure it is not caused by an omission or oversight 25 ALERT level G = General information/check it is not something unexpected 17 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 20 ALERT type 2 Indicator that the structure model may be wrong or deficient 12 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 4 ALERT type 5 Informative message, check
Datablock: Ni_DFT

Alert level A EXPT001_ALERT_1_A _exptl_crystal_density_diffrn is missing Density calculated from unit cell and contents (Mg m-3). The following tests will not be performed. DENSD_01,DENSX_01 DIFF001_ALERT_1_A _diffrn_radiation_type is missing The radiation type should contain one of the following * 'Cu K\a' * 'Mo K\a' * 'Ag K\a' * neutron * synchrotron The following tests will not be performed. ABSMU_01,ABSTM_02,CRYSS_01,RADNW_01 DIFF002_ALERT_1_A _diffrn_radiation_wavelength is missing Radiation wavelength (A). The following tests will not be performed. RADNW_01,REFLT_03,REFNR_01,THETM_01 CELL003_ALERT_1_A _cell_measurement_reflns_used is missing Number of reflections used to measure unit cell. CELL004_ALERT_1_A _cell_measurement_theta_min is missing Minimum theta of reflections used to measure unit cell. The following tests will not be performed. CELLT_01 CELL005_ALERT_1_A _cell_measurement_theta_max is missing Maximum theta of reflections used to measure unit cell. The following tests will not be performed. CELLT_01 CELL006_ALERT_1_A _cell_measurement_temperature is missing Measurement temperature (K). The following tests will not be performed. CELLK_01 EXPT004_ALERT_1_A _exptl_absorpt_coefficient_mu is missing Linear absorption coefficient (mm-1). The following tests will not be performed. ABSMU_01,ABSTM_02 EXPT005_ALERT_1_A _exptl_crystal_description is missing Crystal habit description. The following tests will not be performed. CRYSR_01 EXPT009_ALERT_1_A No crystal dimensions have been given. The following tests will not be performed. CRYSS_01,CRYSS_02 EXPT010_ALERT_1_A _exptl_crystal_colour (_pd_char_colour for powder) is missing Crystal colour. The following tests will not be performed. CRYSC_01 DIFF003_ALERT_1_A _diffrn_measurement_device_type is missing Diffractometer make and type. Replaces _diffrn_measurement_type. DIFF005_ALERT_1_A _diffrn_measurement_method is missing Mode of intensity measurement and scan. DIFF007_ALERT_1_A _diffrn_reflns_number is missing Total number of reflections measured. The following tests will not be performed. REFLG_01,REFLT_01 REFL001_ALERT_1_A _reflns_number_total is missing Number of symmetry-independent reflections. The following tests will not be performed. REFLT_01,REFLT_02,REFLT_03,REFNR_01 REFL002_ALERT_1_A _reflns_number_gt is missing Number of reflections > sigma threshold. The following tests will not be performed. REFLG_01,REFLT_02 REFL004_ALERT_1_A _reflns_threshold_expression is missing Sigma expression for F, F2 or I threshold. The following tests will not be performed. REFLE_01 DIFF008_ALERT_1_A _diffrn_reflns_theta_max is missing Maximum theta of measured reflections. The following tests will not be performed REFLT_03,REFNR_01,THETM_01 DIFF012_ALERT_1_A _diffrn_reflns_av_R_equivalents is missing R factor for symmetry-equivalent intensities. The following tests will not be performed RINTA DIFF013_ALERT_1_A _diffrn_reflns_limit_h_min is missing Minimum h index of measured data. The following tests will not be performed REFLL_01 DIFF014_ALERT_1_A _diffrn_reflns_limit_h_max is missing Maximum h index of measured data. The following tests will not be performed REFLL_01 DIFF015_ALERT_1_A _diffrn_reflns_limit_k_min is missing Minimum k index of measured data. The following tests will not be performed REFLL_01 DIFF016_ALERT_1_A _diffrn_reflns_limit_k_max is missing Maximum k index of measured data. The following tests will not be performed REFLL_01 DIFF017_ALERT_1_A _diffrn_reflns_limit_l_min is missing Minimum l index of measured data. The following tests will not be performed REFLL_01 DIFF018_ALERT_1_A _diffrn_reflns_limit_l_max is missing Maximum l index of measured data. The following tests will not be performed REFLL_01 DIFF019_ALERT_1_A _diffrn_standards_number is missing Number of standards used in measurement. DIFF020_ALERT_1_A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards. DIFF022_ALERT_1_A _diffrn_standards_decay_% is missing Percentage decrease in standards intensity. REFI001_ALERT_1_A _refine_ls_structure_factor_coef is missing The structure factor coefficient should be one of the following * Inet * Fsqd * F The following tests will not be performed FCOEF_01 REFI003_ALERT_1_A _refine_ls_R_factor_gt is missing R factor of F for reflections > threshold. The following tests will not be performed RFACG_01 REFI005_ALERT_1_A _refine_ls_wR_factor_ref is missing R factor of coefficient for refinement reflections. The following tests will not be performed RFACR_01 REFI007_ALERT_1_A _refine_ls_goodness_of_fit_ref is missing Goodness of fit S for refinement reflections. The following tests will not be performed GOODF_01 REFI009_ALERT_1_A _refine_ls_number_reflns is missing Number of reflections used in refinement. The following test will not be performed REFNR_01 REFI010_ALERT_1_A _refine_ls_number_parameters is missing Number of parameters refined. The following tests will not be performed REFNR_01 REFI011_ALERT_1_A _refine_ls_weighting_scheme is missing The weighting scheme should be one of the following * sigma * calc The following tests will not be performed WEIGH_01 REFI014_ALERT_1_G _refine_ls_hydrogen_treatment is missing Code for H-atom treatment. The following tests will not be performed HYDTR_01 REFI015_ALERT_1_C _refine_ls_shift/su_max is missing Maximum shift/s.u. ratio after final refinement cycle. The following tests will not be performed SHFSU_01 REFI017_ALERT_1_A _refine_diff_density_max is missing Maximum value of final difference map (e A-3). The following tests will not be performed DIFMN_01,DIFMX_01,DIFMX_02 REFI018_ALERT_1_A _refine_diff_density_min is missing Minimum value of final difference map (e A-3). The following tests will not be performed DIFMN_01,DIFMN_02,DIFMN_03 ATOM006_ALERT_1_A _atom_site_U_iso_or_equiv is missing Isotropic atomic displacement paramter, or equivalent from anisotropic atomic displacement parameters. ATOM007_ALERT_1_A _atom_site_aniso_label is missing Unique label identifying the atom site. GEOM001_ALERT_1_A _geom_bond_atom_site_label_1 is missing Label identifying the atom site 1. GEOM002_ALERT_1_A _geom_bond_atom_site_label_2 is missing Label identifying the atom site 2. GEOM003_ALERT_1_A _geom_bond_distance is missing Distance between atom sites 1 and 2. PLAT039_ALERT_1_A _diffrn_measured_fraction_theta_full Not Given . Please Do ! PLAT044_ALERT_1_A Calculated and Reported Density Dx Differ by .. 1.8930 Check PLAT183_ALERT_1_A Missing _cell_measurement_reflns_used Value .... Please Do ! PLAT184_ALERT_1_A Missing _cell_measurement_theta_min Value ...... Please Do ! PLAT185_ALERT_1_A Missing _cell_measurement_theta_max Value ...... Please Do ! PLAT197_ALERT_1_A Missing _cell_measurement_temperature Datum .... Please Add PLAT198_ALERT_1_A Missing _diffrn_ambient_temperature Datum .... Please Add PLAT699_ALERT_1_A Missing _exptl_crystal_description Value ....... Please Do ! PLAT880_ALERT_1_A No datum for _diffrn_reflns_number supplied .... Please Do ! PLAT881_ALERT_1_A No Datum for _diffrn_reflns_av_R_equivalents ... Please Do !
Alert level B PLAT420_ALERT_2_B D-H Bond Without Acceptor O16 --H17 . Please Check
Alert level C PLAT141_ALERT_4_C s.u. on a - Axis Small or Missing .............. 0.00000 Ang. PLAT142_ALERT_4_C s.u. on b - Axis Small or Missing .............. 0.00000 Ang. PLAT143_ALERT_4_C s.u. on c - Axis Small or Missing .............. 0.00000 Ang. PLAT144_ALERT_4_C s.u. on alpha Small or Missing .............. 0.0000 Degree PLAT145_ALERT_4_C s.u. on beta Small or Missing .............. 0.0000 Degree PLAT146_ALERT_4_C s.u. on gamma Small or Missing .............. 0.0000 Degree PLAT151_ALERT_1_C No s.u. (esd) Given on Volume .................. Please Do ! PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced .......... Please Do ! PLAT410_ALERT_2_C Short Intra H...H Contact H2 ..H9 . 1.94 Ang. 1-x,1-y,-z = 2_665 Check PLAT761_ALERT_1_C CIF Contains no X-H Bonds ...................... Please Check PLAT762_ALERT_1_C CIF Contains no X-Y-H or H-Y-H Angles .......... Please Check
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C14 H10 Ni2 O6 Atom count from _chemical_formula_moiety:C7 H5 Ni1 O3 PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension 2 Info PLAT005_ALERT_5_G No Embedded Refinement Details Found in the CIF Please Do ! PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 1 Report PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... 2 Check PLAT794_ALERT_5_G Tentative Bond Valency for Ni14 (II) . 1.92 Info PLAT794_ALERT_5_G Tentative Bond Valency for Ni15 (III) . 2.95 Info PLAT808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found Please Check PLAT882_ALERT_1_G No Datum for _diffrn_reflns_av_unetI/netI ...... Please Do ! PLAT883_ALERT_1_G No Info/Value for _atom_sites_solution_primary . Please Do ! PLAT980_ALERT_1_G No Anomalous Scattering Factors Found in CIF ... Please Check
52 ALERT level A = Most likely a serious problem - resolve or explain 1 ALERT level B = A potentially serious problem, consider carefully 12 ALERT level C = Check. Ensure it is not caused by an omission or oversight 12 ALERT level G = General information/check it is not something unexpected 62 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 7 ALERT type 4 Improvement, methodology, query or suggestion 6 ALERT type 5 Informative message, check
Datablock: NH4_X

Alert level A PLAT080_ALERT_2_A Maximum Shift/Error ............................ 0.72 Why ? PLAT411_ALERT_2_A Short Inter H...H Contact H9 ..H18 . 1.67 Ang. x,1+y,z = 1_565 Check PLAT417_ALERT_2_A Short Inter D-H..H-D H30 ..H36 . 1.67 Ang. -1+x,y,z = 1_455 Check PLAT430_ALERT_2_A Short Inter D...A Contact O23 ..O25 . 2.48 Ang. -1+x,y,z = 1_455 Check
Alert level B PLAT340_ALERT_3_B Low Bond Precision on C-C Bonds ............... 0.0344 Ang. PLAT417_ALERT_2_B Short Inter D-H..H-D H30 ..H35 . 2.05 Ang. -1+x,y,z = 1_455 Check
Alert level C PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ Please Check PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C21 Check PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C22 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C6 Check PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of C12 Check PLAT309_ALERT_2_C Single Bonded Oxygen (C-O > 1.3 Ang) ........... O25 Check PLAT334_ALERT_2_C Small <C-C> Benzene Dist. C2 -C5 . 1.36 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C2 - H1 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C3 - H10 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C5 - H8 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C7 - H9 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C13 - H17 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C14 - H18 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C15 - H19 . 1.14 Ang. PLAT351_ALERT_3_C Long C-H (X0.96,N1.08A) C16 - H20 . 1.14 Ang. PLAT353_ALERT_3_C Long N-H (N0.87,N1.01A) N28 - H33 . 1.03 Ang. PLAT353_ALERT_3_C Long N-H (N0.87,N1.01A) N28 - H34 . 1.03 Ang. PLAT353_ALERT_3_C Long N-H (N0.87,N1.01A) N28 - H35 . 1.03 Ang. PLAT353_ALERT_3_C Long N-H (N0.87,N1.01A) N27 - H29 . 1.03 Ang. PLAT353_ALERT_3_C Long N-H (N0.87,N1.01A) N27 - H30 . 1.05 Ang. PLAT353_ALERT_3_C Long N-H (N0.87,N1.01A) N27 - H31 . 1.03 Ang. PLAT353_ALERT_3_C Long N-H (N0.87,N1.01A) N27 - H32 . 1.03 Ang. PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C12 - C21 . 1.55 Ang. PLAT411_ALERT_2_C Short Inter H...H Contact H1 ..H18 . 2.03 Ang. -1+x,y,z = 1_455 Check PLAT420_ALERT_2_C D-H Bond Without Acceptor N28 --H34 . Please Check PLAT420_ALERT_2_C D-H Bond Without Acceptor N28 --H35 . Please Check
Alert level G PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 8 Report PLAT092_ALERT_4_G Check: Wavelength Given is not Cu,Ga,Mo,Ag,In Ka 0.71361 Ang. PLAT303_ALERT_2_G Full Occupancy Atom H36 with # Connections 2.00 Check PLAT343_ALERT_2_G Unusual sp? Angle Range in Main Residue for C22 Check PLAT367_ALERT_2_G Long? C(sp?)-C(sp?) Bond C6 - C22 . 1.52 Ang. PLAT432_ALERT_2_G Short Inter X...Y Contact N27 ..C22 . 2.81 Ang. -1+x,y,z = 1_455 Check PLAT721_ALERT_1_G Bond Calc 1.05000, Rep 1.02944 Dev... 0.02 Ang. N27 -H30 1_555 1_555 ........ # 40 Check PLAT721_ALERT_1_G Bond Calc 1.05000, Rep 1.02944 Dev... 0.02 Ang. H30 -N27 1_555 1_555 ........ # 44 Check PLAT722_ALERT_1_G Angle Calc 108.00, Rep 109.48 Dev... 1.48 Degree H29 -N27 -H30 1_555 1_555 1_555 # 27 Check PLAT722_ALERT_1_G Angle Calc 111.00, Rep 109.47 Dev... 1.53 Degree H30 -N27 -H32 1_555 1_555 1_555 # 31 Check PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 2.00 Ratio PLAT769_ALERT_4_G CIF Embedded explicitly supplied scattering data Please Note PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 2 Note H4 N PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 55 Note
4 ALERT level A = Most likely a serious problem - resolve or explain 2 ALERT level B = A potentially serious problem, consider carefully 26 ALERT level C = Check. Ensure it is not caused by an omission or oversight 14 ALERT level G = General information/check it is not something unexpected 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 19 ALERT type 2 Indicator that the structure model may be wrong or deficient 17 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
checkCIF publication errors
Alert level A PUBL003_ALERT_1_A The contact author's name is missing, _publ_contact_author_name. PUBL006_ALERT_1_A _publ_requested_journal is missing e.g. 'Acta Crystallographica Section C'
2 ALERT level A = Data missing that is essential or data in wrong format 0 ALERT level G = General alerts. Data that may be required is missing # start Validation Reply Form _vrf_PUBL003_GLOBAL ; PROBLEM: The contact author's name is missing, RESPONSE: ... ; _vrf_PUBL006_GLOBAL ; PROBLEM: _publ_requested_journal is missing RESPONSE: ... ; _vrf_PLAT080_Co_X ; PROBLEM: Maximum Shift/Error ............................ 2.59 Why ? RESPONSE: ... ; _vrf_PLAT701_Co_X ; PROBLEM: Bond Calc 16.07(6), Rep 2.105(9), Dev.. 232.75 Sigma RESPONSE: ... ; _vrf_CELLV01_Ni_X ; PROBLEM: The supplied cell volume differs from that calculated from RESPONSE: ... ; _vrf_PLAT080_Ni_X ; PROBLEM: Maximum Shift/Error ............................ 4.43 Why ? RESPONSE: ... ; _vrf_PLAT341_Ni_X ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.16375 Ang. RESPONSE: ... ; _vrf_PLAT701_Ni_X ; PROBLEM: Bond Calc 15.8(12), Rep 1.953(12), Dev.. 11.54 Sigma RESPONSE: ... ; _vrf_EXPT001_Ni_DFT ; PROBLEM: _exptl_crystal_density_diffrn is missing RESPONSE: ... ; _vrf_DIFF001_Ni_DFT ; PROBLEM: _diffrn_radiation_type is missing RESPONSE: ... ; _vrf_DIFF002_Ni_DFT ; PROBLEM: _diffrn_radiation_wavelength is missing RESPONSE: ... ; _vrf_CELL003_Ni_DFT ; PROBLEM: _cell_measurement_reflns_used is missing RESPONSE: ... ; _vrf_CELL004_Ni_DFT ; PROBLEM: _cell_measurement_theta_min is missing RESPONSE: ... ; _vrf_CELL005_Ni_DFT ; PROBLEM: _cell_measurement_theta_max is missing RESPONSE: ... ; _vrf_CELL006_Ni_DFT ; PROBLEM: _cell_measurement_temperature is missing RESPONSE: ... ; _vrf_EXPT004_Ni_DFT ; PROBLEM: _exptl_absorpt_coefficient_mu is missing RESPONSE: ... ; _vrf_EXPT005_Ni_DFT ; PROBLEM: _exptl_crystal_description is missing RESPONSE: ... ; _vrf_EXPT009_Ni_DFT ; PROBLEM: No crystal dimensions have been given. RESPONSE: ... ; _vrf_EXPT010_Ni_DFT ; PROBLEM: _exptl_crystal_colour (_pd_char_colour for powder) is missing RESPONSE: ... ; _vrf_DIFF003_Ni_DFT ; PROBLEM: _diffrn_measurement_device_type is missing RESPONSE: ... ; _vrf_DIFF005_Ni_DFT ; PROBLEM: _diffrn_measurement_method is missing RESPONSE: ... ; _vrf_DIFF007_Ni_DFT ; PROBLEM: _diffrn_reflns_number is missing RESPONSE: ... ; _vrf_REFL001_Ni_DFT ; PROBLEM: _reflns_number_total is missing RESPONSE: ... ; _vrf_REFL002_Ni_DFT ; PROBLEM: _reflns_number_gt is missing RESPONSE: ... ; _vrf_REFL004_Ni_DFT ; PROBLEM: _reflns_threshold_expression is missing RESPONSE: ... ; _vrf_DIFF008_Ni_DFT ; PROBLEM: _diffrn_reflns_theta_max is missing RESPONSE: ... ; _vrf_DIFF012_Ni_DFT ; PROBLEM: _diffrn_reflns_av_R_equivalents is missing RESPONSE: ... ; _vrf_DIFF013_Ni_DFT ; PROBLEM: _diffrn_reflns_limit_h_min is missing RESPONSE: ... ; _vrf_DIFF014_Ni_DFT ; PROBLEM: _diffrn_reflns_limit_h_max is missing RESPONSE: ... ; _vrf_DIFF015_Ni_DFT ; PROBLEM: _diffrn_reflns_limit_k_min is missing RESPONSE: ... ; _vrf_DIFF016_Ni_DFT ; PROBLEM: _diffrn_reflns_limit_k_max is missing RESPONSE: ... ; _vrf_DIFF017_Ni_DFT ; PROBLEM: _diffrn_reflns_limit_l_min is missing RESPONSE: ... ; _vrf_DIFF018_Ni_DFT ; PROBLEM: _diffrn_reflns_limit_l_max is missing RESPONSE: ... ; _vrf_DIFF019_Ni_DFT ; PROBLEM: _diffrn_standards_number is missing RESPONSE: ... ; _vrf_DIFF020_Ni_DFT ; PROBLEM: _diffrn_standards_interval_count and RESPONSE: ... ; _vrf_DIFF022_Ni_DFT ; PROBLEM: _diffrn_standards_decay_% is missing RESPONSE: ... ; _vrf_REFI001_Ni_DFT ; PROBLEM: _refine_ls_structure_factor_coef is missing RESPONSE: ... ; _vrf_REFI003_Ni_DFT ; PROBLEM: _refine_ls_R_factor_gt is missing RESPONSE: ... ; _vrf_REFI005_Ni_DFT ; PROBLEM: _refine_ls_wR_factor_ref is missing RESPONSE: ... ; _vrf_REFI007_Ni_DFT ; PROBLEM: _refine_ls_goodness_of_fit_ref is missing RESPONSE: ... ; _vrf_REFI009_Ni_DFT ; PROBLEM: _refine_ls_number_reflns is missing RESPONSE: ... ; _vrf_REFI010_Ni_DFT ; PROBLEM: _refine_ls_number_parameters is missing RESPONSE: ... ; _vrf_REFI011_Ni_DFT ; PROBLEM: _refine_ls_weighting_scheme is missing RESPONSE: ... ; _vrf_REFI017_Ni_DFT ; PROBLEM: _refine_diff_density_max is missing RESPONSE: ... ; _vrf_REFI018_Ni_DFT ; PROBLEM: _refine_diff_density_min is missing RESPONSE: ... ; _vrf_ATOM006_Ni_DFT ; PROBLEM: _atom_site_U_iso_or_equiv is missing RESPONSE: ... ; _vrf_ATOM007_Ni_DFT ; PROBLEM: _atom_site_aniso_label is missing RESPONSE: ... ; _vrf_GEOM001_Ni_DFT ; PROBLEM: _geom_bond_atom_site_label_1 is missing RESPONSE: ... ; _vrf_GEOM002_Ni_DFT ; PROBLEM: _geom_bond_atom_site_label_2 is missing RESPONSE: ... ; _vrf_GEOM003_Ni_DFT ; PROBLEM: _geom_bond_distance is missing RESPONSE: ... ; _vrf_PLAT039_Ni_DFT ; PROBLEM: _diffrn_measured_fraction_theta_full Not Given . Please Do ! RESPONSE: ... ; _vrf_PLAT044_Ni_DFT ; PROBLEM: Calculated and Reported Density Dx Differ by .. 1.8930 Check RESPONSE: ... ; _vrf_PLAT183_Ni_DFT ; PROBLEM: Missing _cell_measurement_reflns_used Value .... Please Do ! RESPONSE: ... ; _vrf_PLAT184_Ni_DFT ; PROBLEM: Missing _cell_measurement_theta_min Value ...... Please Do ! RESPONSE: ... ; _vrf_PLAT185_Ni_DFT ; PROBLEM: Missing _cell_measurement_theta_max Value ...... Please Do ! RESPONSE: ... ; _vrf_PLAT197_Ni_DFT ; PROBLEM: Missing _cell_measurement_temperature Datum .... Please Add RESPONSE: ... ; _vrf_PLAT198_Ni_DFT ; PROBLEM: Missing _diffrn_ambient_temperature Datum .... Please Add RESPONSE: ... ; _vrf_PLAT699_Ni_DFT ; PROBLEM: Missing _exptl_crystal_description Value ....... Please Do ! RESPONSE: ... ; _vrf_PLAT880_Ni_DFT ; PROBLEM: No datum for _diffrn_reflns_number supplied .... Please Do ! RESPONSE: ... ; _vrf_PLAT881_Ni_DFT ; PROBLEM: No Datum for _diffrn_reflns_av_R_equivalents ... Please Do ! RESPONSE: ... ; _vrf_PLAT080_NH4_X ; PROBLEM: Maximum Shift/Error ............................ 0.72 Why ? RESPONSE: ... ; _vrf_PLAT411_NH4_X ; PROBLEM: Short Inter H...H Contact H9 ..H18 . 1.67 Ang. RESPONSE: ... ; _vrf_PLAT417_NH4_X ; PROBLEM: Short Inter D-H..H-D H30 ..H36 . 1.67 Ang. RESPONSE: ... ; _vrf_PLAT430_NH4_X ; PROBLEM: Short Inter D...A Contact O23 ..O25 . 2.48 Ang. RESPONSE: ... ; # end Validation Reply Form

Computing details top

Program(s) used to solve structure: DFT for Co_DFT, NH4_DFT. Program(s) used to refine structure: GSAS-II (Toby & Von Dreele, 2013) for Co_X, Ni_X, NH4_X.

Poly[(µ4-4,4'-biphenyldicarboxylato)di-µ-hydroxido-dicobalt] (Co_X) top
Crystal data top
[Co(C14H8O4)0.5(OH)]β = 98.46 (7)°
Mr = 392.09γ = 90.0 (3)°
Triclinic, P1V = 291.6 (2) Å3
Hall symbol: -P 1Z = 1
a = 14.16 (5) ÅDx = 2.233 Mg m3
b = 6.269 (3) Å Kα1,2 radiation, λ = 0.70932, 0.71361 Å
c = 3.323 (4) ÅT = 300 K
α = 91.43 (2)°cylinder, 12 × 0.7 mm
Data collection top
PANalytical Empyrean
diffractometer
Scan method: step
Specimen mounting: glass capillary2θmin = 1.002°, 2θmax = 49.991°, 2θstep = 0.008°
Data collection mode: transmission
Refinement top
Least-squares matrix: fullProfile function: Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L: peak variance(Gauss) = Utan(Th)2+Vtan(Th)+W: peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L U, V, W in (centideg)2, X & Y in centideg 30.816, 10.768, 0.000, 1.935, 0.000, 0.033,
Rp = 0.06549 parameters
Rwp = 0.092H-atom parameters not defined?
Rexp = 0.022(Δ/σ)max = 2.587
R(F2) = 0.11340Background function: Background function: "chebyschev-1" function with 4 terms: 1205(8), -655(9), 147(7), -88(6), Background peak parameters: pos, int, sig, gam: 11.72(4), 4.94(12)e5, 3.12(13)e4, 0.100,
5864 data pointsPreferred orientation correction: March-Dollase correction coef. = 1.000 axis = [0, 0, 1]
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.613 (3)0.625 (7)0.90 (3)0.26 (3)*
C30.704 (3)0.560 (8)0.84 (3)0.26 (3)*
C50.7409 (16)0.364 (3)0.97 (2)0.26 (3)*
C60.688 (3)0.233 (7)1.18 (3)0.26 (3)*
C80.594 (3)0.287 (11)1.23 (2)0.26 (3)*
C100.5516 (10)0.485 (9)1.077 (11)0.26 (3)*
C110.8397 (9)0.301 (2)0.895 (13)0.026 (13)*
O120.8581 (8)0.108 (3)0.890 (6)0.026 (13)*
O130.9031 (7)0.446 (2)0.938 (3)0.026 (13)*
H20.586660.795550.810880.3419*
H40.750030.668820.674010.3419*
H70.720540.079821.314270.3419*
H90.549820.174041.389760.3419*
O160.9611 (9)0.8112 (12)0.471 (3)0.0500*
H170.890310.810570.422720.0650*
Co141.000000.000001.000000.018 (3)*
Co151.000000.500000.500000.018 (3)*
Geometric parameters (Å, º) top
C1—C31.399 (18)O12—C111.232 (10)
C1—C101.427 (15)O12—Co142.105 (9)
C3—C11.399 (18)O13—C111.272 (11)
C3—C51.389 (7)O16—H170.992 (13)
C5—C31.389 (7)O16—Co14ii2.098 (8)
C5—C61.385 (8)O16—Co14iii2.121 (8)
C5—C111.503 (8)O16—Co152.028 (8)
C6—C51.385 (8)H17—O160.992 (13)
C6—C81.41 (3)Co14—O122.105 (9)
C8—C61.41 (3)Co14—O12iv2.105 (9)
C8—C101.447 (15)Co14—O16v2.121 (8)
C10—C11.427 (15)Co14—O16vi2.098 (8)
C10—C81.447 (15)Co14—O16vii2.098 (8)
C10—C10i1.489 (5)Co14—O16viii2.121 (8)
C11—C51.503 (8)Co15—O162.028 (8)
C11—O121.232 (10)Co15—O16viii2.028 (8)
C11—O131.272 (11)
C3—C1—C10121.0 (6)C1—C10—C8116.0 (9)
C1—C3—C5121.4 (5)C1—C10—C10i114 (5)
C3—C5—C6119.5 (5)C8—C10—C10i124 (6)
C3—C5—C11119.9 (5)C5—C11—O12117.3 (8)
C6—C5—C11120.5 (6)C5—C11—O13117.1 (8)
C5—C6—C8120.5 (9)O12—C11—O13123.6 (10)
C6—C8—C10120.9 (10)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+1, z; (iii) x, y+1, z1; (iv) x+2, y, z+2; (v) x, y1, z+1; (vi) x, y1, z; (vii) x+2, y+1, z+2; (viii) x+2, y+1, z+1.
(Co_DFT) top
Crystal data top
C14H10Co2O6α = 91.80°
Mr = 392.09β = 99.44°
Triclinic, P1γ = 89.98°
a = 14.20000 ÅV = 302.23 Å3
b = 6.23720 ÅZ = 1
c = 3.46100 Å
Data collection top
h = l =
k =
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
C10.615690.620160.89476
C30.709730.565350.88026
C50.740570.354980.94939
C60.676010.203381.04253
C80.582790.260431.06503
C100.549780.470000.98891
C110.840120.290620.92724
O120.858730.092060.91494
O130.902990.440770.92824
H20.593610.784130.83081
H40.760000.684830.81104
H70.701190.041011.10392
H90.535430.139711.15004
O160.959810.195910.47462
H170.890310.189430.42272
Co141.000000.000001.00000
Co151.000000.500000.50000
Poly[(µ4-4,4'-biphenyldicarboxylato)di-µ-hydroxido-dinickel] (Ni_X) top
Crystal data top
[Ni(C14H8O4)0.5(OH)]β = 72.3 (8)°
Mr = 391.63γ = 82 (2)°
Triclinic, P1V = 345 (2) Å3
Hall symbol: -P 1Z = 1
a = 15.0 (11) ÅDx = 1.883 Mg m3
b = 6.04 (12) Å Kα1,2 radiation, λ = 1.54059, 1.54445 Å
c = 4.04 (9) ÅT = 300 K
α = 82.7 (2)°flat_sheet, 16 × 16 mm
Data collection top
PANalytical X'Pert
diffractometer
Scan method: step
Specimen mounting: Si zero-background cell with well2θmin = 4.008°, 2θmax = 99.998°, 2θstep = 0.017°
Data collection mode: reflection
Refinement top
Least-squares matrix: full47 parameters
Rp = 0.04230 restraints
Rwp = 0.059H-atom parameters not defined?
Rexp = 0.011(Δ/σ)max = 4.433
R(F2) = 0.09176Background function: Background function: "chebyschev-1" function with 6 terms: 6.12(5)e3, -3.68(4)e3, 8.6(4)e2, 83(31), -134(21), 50(21),
5745 data pointsPreferred orientation correction: March-Dollase correction coef. = 1.000 axis = [0, 0, 1]
Profile function: Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L: peak variance(Gauss) = Utan(Th)2+Vtan(Th)+W: peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L U, V, W in (centideg)2, X & Y in centideg 5.186, -8.449, 5.755, 3.463, 0.000, 0.021,
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.620 (3)0.56 (4)0.23 (3)0.02 (4)*
C30.707 (2)0.51 (2)0.21 (3)0.02 (4)*
C50.7272 (18)0.38 (2)0.07 (2)0.02 (4)*
C60.653 (4)0.30 (3)0.34 (3)0.02 (4)*
C80.568 (2)0.322 (18)0.32 (2)0.02 (4)*
C100.546 (3)0.46 (3)0.02 (4)0.02 (4)*
C110.8370 (16)0.350 (15)0.074 (19)0.2200*
O120.873 (4)0.147 (19)0.13 (5)0.2200*
O130.897 (4)0.50 (2)0.066 (13)0.2200*
H20.603690.683680.444990.0500*
H40.767080.580560.438090.0500*
H70.666730.2101110.588220.0500*
H90.510340.2339930.524870.0500*
Ni141.000000.000000.000000.018 (14)*
O161.00 (2)0.179 (4)0.43 (2)0.1000*
H170.938290.171840.502340.1300*
Ni151.000000.500000.500000.018 (14)*
Geometric parameters (Å, º) top
C1—C31.31 (2)C11—O131.311 (16)
C1—C101.39 (3)O12—C111.297 (10)
C3—C11.31 (2)O12—Ni141.942 (14)
C3—C51.396 (9)O13—C111.311 (16)
C5—C31.396 (9)O13—Ni151.953 (12)
C5—C61.404 (16)Ni14—O121.942 (14)
C5—C111.642 (12)Ni14—O12ii1.942 (14)
C6—C51.404 (16)Ni14—O161.927 (19)
C6—C81.31 (2)Ni14—O16ii1.927 (19)
C8—C61.31 (2)O16—Ni141.927 (19)
C8—C101.46 (2)O16—Ni15ii1.919 (13)
C10—C11.39 (3)Ni15—O131.953 (12)
C10—C81.46 (2)Ni15—O13iii1.953 (12)
C10—C10i1.464 (8)Ni15—O16iv1.919 (13)
C11—C51.642 (12)Ni15—O16ii1.919 (13)
C11—O121.297 (10)
C3—C1—C10122 (2)C1—C10—C8117.5 (18)
C1—C3—C5120.8 (6)C1—C10—C10i114 (5)
C3—C5—C6119.0 (9)C8—C10—C10i128 (8)
C5—C6—C8120.9 (19)O12—C11—O13115.7 (12)
C6—C8—C10119.7 (8)
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y, z; (iii) x+2, y+1, z1; (iv) x, y+1, z1.
(Ni_DFT) top
Crystal data top
C14H10Ni2O6α = 81.57°
Mr = 391.63β = 71.90°
Triclinic, P1γ = 81.90°
a = 15.10000 ÅV = 343.52 Å3
b = 6.05000 ÅZ = 1
c = 4.02000 Å
Data collection top
h = l =
k =
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
C10.611470.636100.07671
C30.703130.583100.06941
C50.736670.362920.03127
C60.673290.199560.14026
C80.581300.253740.13082
C100.548110.471970.01398
C110.839070.311160.01437
O120.871530.111940.07915
O130.886250.478670.15724
H20.589880.809140.16146
H40.751090.712750.14925
H70.697100.028210.22559
H90.534780.120630.21394
Ni141.000000.000000.00000
O160.964160.189430.44560
H170.896730.166840.55127
Ni151.000000.500000.50000
(UBUPEQ_DFT) top
Crystal data top
C14H10Mn2O6α = 90.09°
Triclinic, P1β = 96.84°
a = 14.20370 Åγ = 91.71°
b = 6.47851 ÅV = 315.35 Å3
c = 3.45320 ÅZ = 2
Data collection top
h = l =
k =
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
C10.620980.613700.92029
H10.603890.774290.86234
C20.714020.557070.91323
H20.767920.672530.85491
C30.739120.351040.97430
C40.669140.205990.05646
H30.689460.047070.11422
C50.576810.264600.07216
H40.525060.148400.14642
C60.549450.469450.99724
C70.836660.284960.94908
O10.852810.094020.92904
O20.903270.428160.95195
Mn11.000000.000000.00000
Mn21.000000.500000.50000
O30.955660.196180.47885
H170.8866190.190370.44315
Diammonium 4,4'-biphenyldicarboxylate (NH4_X) top
Crystal data top
2NH4+·C14H8O42β = 91.41 (4)°
Mr = 276.29γ = 92.775 (11)°
Triclinic, P1V = 351.43 (17) Å3
Hall symbol: P 1Z = 1
a = 4.6770 (6) ÅDx = 1.306 Mg m3
b = 5.2306 (14) Å Kα1,2 radiation, λ = 0.70932, 0.71361 Å
c = 14.387 (6) ÅT = 300 K
α = 90.57 (7)°cylinder, 12 × 0.7 mm
Data collection top
PANalytical Empyrean
diffractometer
Scan method: step
Specimen mounting: glass capillary2θmin = 1.008°, 2θmax = 49.982°, 2θstep = 0.008°
Data collection mode: transmission
Refinement top
Least-squares matrix: full93 parameters
Rp = 0.03355 restraints
Rwp = 0.043H-atom parameters not defined?
Rexp = 0.015(Δ/σ)max = 0.723
R(F2) = 0.09394Background function: Background function: "chebyschev-1" function with 4 terms: 3149(17), -491(16), 99(12), -147(15), Background peak parameters: pos, int, sig, gam: 12.38(8), 1.18(6)e6, 1.20(8)e5, 0.100,
5862 data pointsPreferred orientation correction: Simple spherical harmonic correction Order = 4 Coefficients: 0:0:C(2,-2) = 0.79(3); 0:0:C(2,-1) = 0.32(7); 0:0:C(2,0) = 0.330(31); 0:0:C(2,1) = 1.58(9); 0:0:C(2,2) = 0.88(4); 0:0:C(4,-4) = 0.33(7); 0:0:C(4,-3) = 1.02(5); 0:0:C(4,-2) = 0.65(6); 0:0:C(4,-1) = -0.39(8); 0:0:C(4,0) = -0.79(4); 0:0:C(4,1) = -0.01(9); 0:0:C(4,2) = 1.10(6); 0:0:C(4,3) = 0.79(8); 0:0:C(4,4) = -0.31(7)
Profile function: Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L: peak variance(Gauss) = Utan(Th)2+Vtan(Th)+W: peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L U, V, W in (centideg)2, X & Y in centideg 30.816, 10.768, 0.000, 1.935, 0.000, 0.033,
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
H10.562710.557480.049030.0500*
C20.726500.710070.072770.0042*
C31.092 (10)1.091 (7)0.1369 (14)0.0042*
C40.886 (5)0.858 (4)0.0073 (7)0.0042*
C50.759 (8)0.741 (7)0.1644 (4)0.0042*
C60.942 (5)0.928 (5)0.1987 (9)0.0042*
C71.068 (8)1.055 (6)0.0421 (13)0.0042*
H80.632740.609980.216060.0500*
H91.196661.185860.009010.0500*
H101.235361.254940.163910.0500*
C110.935 (5)0.754 (5)0.0884 (8)0.0042*
C121.040 (7)0.578 (6)0.2730 (11)0.0042*
C130.788 (12)0.847 (10)0.1638 (15)0.0042*
C141.140 (8)0.571 (9)0.1072 (12)0.0042*
C151.197 (11)0.490 (10)0.1986 (15)0.0042*
C160.833 (10)0.754 (9)0.2538 (12)0.0042*
H170.627411.001790.152950.0500*
H181.263050.485830.047870.0500*
H191.373640.350940.211560.0500*
H200.695280.825860.311940.0500*
C211.076 (7)0.480 (7)0.3737 (13)0.0566*
C220.944 (5)0.962 (6)0.3033 (10)0.0566*
O230.840 (7)0.413 (8)0.4081 (17)0.0566*
O240.969 (10)0.758 (7)0.3508 (14)0.0566*
O251.309 (7)0.371 (8)0.4015 (16)0.0566*
O260.762 (7)1.119 (7)0.3310 (18)0.0566*
N270.344751.288360.391680.0500*
H290.360011.439310.436950.0500*
H300.228781.137560.426060.0500*
H310.546821.232370.374050.0500*
H320.243381.344220.332650.0500*
N280.887140.855880.477160.0500*
H330.850370.660620.482790.0500*
H340.696090.944310.484490.0500*
H351.023200.917380.528390.0500*
H360.978930.901220.412980.0500*
Geometric parameters (Å, º) top
C2—C41.392 (7)C16—C131.402 (7)
C2—C51.342 (6)C21—C121.550 (7)
C3—C61.379 (6)C21—O231.258 (9)
C3—C71.385 (6)C21—O251.310 (9)
C4—C21.392 (7)C22—C61.518 (7)
C4—C71.408 (7)C22—O241.269 (9)
C4—C111.501 (8)C22—O261.272 (9)
C5—C21.342 (6)O23—C211.258 (9)
C5—C61.373 (6)O24—C221.269 (9)
C6—C31.379 (6)O25—C211.310 (9)
C6—C51.373 (6)O26—C221.272 (9)
C6—C221.518 (7)N27—H291.0294
C7—C31.385 (6)N27—H301.0294
C7—C41.408 (7)N27—H311.0295
C11—C41.501 (8)N27—H321.0294
C11—C131.394 (8)H29—N271.0294
C11—C141.410 (7)H30—N271.0294
C12—C151.401 (6)H31—N271.0295
C12—C161.390 (6)H32—N271.0294
C12—C211.550 (7)N28—H331.0295
C13—C111.394 (8)N28—H341.0295
C13—C161.402 (7)N28—H351.0294
C14—C111.410 (7)N28—H361.0293
C14—C151.408 (6)H33—N281.0295
C15—C121.401 (6)H34—N281.0295
C15—C141.408 (6)H35—N281.0294
C16—C121.390 (6)H36—N281.0293
C4—C2—C5121.9 (4)C12—C16—C13121.6 (3)
C6—C3—C7119.9 (3)C12—C21—O23111.9 (7)
C2—C4—C7116.5 (4)C12—C21—O25121.5 (7)
C2—C4—C11119.4 (6)O23—C21—O25119.6 (8)
C7—C4—C11120.9 (6)C6—C22—O24115.6 (7)
C2—C5—C6121.7 (3)C6—C22—O26112.0 (7)
C3—C6—C5118.8 (4)O24—C22—O26118.2 (8)
C3—C6—C22123.5 (5)H29—N27—H30109.483
C5—C6—C22117.4 (5)H29—N27—H31109.476
C3—C7—C4121.0 (4)H30—N27—H31109.464
C4—C11—C13120.6 (5)H29—N27—H32109.459
C4—C11—C14122.2 (5)H30—N27—H32109.468
C13—C11—C14117.1 (4)H31—N27—H32109.477
C15—C12—C16117.7 (3)H33—N28—H34109.48
C15—C12—C21123.1 (4)H33—N28—H35109.471
C16—C12—C21119.1 (4)H34—N28—H35109.47
C11—C13—C16121.4 (6)H33—N28—H36109.475
C11—C14—C15121.2 (4)H34—N28—H36109.469
C12—C15—C14120.8 (4)H35—N28—H36109.461
(NH4_DFT) top
Crystal data top
C14H16N2O4α = 90.7300°
Mr = 276.29β = 91.3790°
Triclinic, P1γ = 92.7400°
a = 4.6875 ÅV = 352.86 Å3
b = 5.2421 ÅZ = 1
c = 14.3820 Å
Data collection top
h = l =
k =
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
H10.594500.550160.047090.0500*
C20.726500.710070.072770.0042*
C31.064021.114460.140040.0042*
C40.921750.841640.011880.0042*
C50.695640.782210.165360.0042*
C60.861130.987740.199520.0042*
C71.092981.041870.047640.0042*
H80.541360.676760.210980.0500*
H91.254071.139990.002420.0500*
H101.202391.269160.166430.0500*
C110.939490.776580.088680.0042*
C120.949510.647590.279100.0042*
C130.781110.910480.153130.0042*
C141.107770.581420.121660.0042*
C151.113870.517920.215430.0042*
C160.784580.845720.246620.0042*
H170.650531.064400.129100.0500*
H181.235680.478520.072780.0500*
H191.243430.364440.240340.0500*
H200.652940.946380.295010.0500*
C210.938570.569000.378980.0566*
C220.833621.073410.298720.0566*
O230.762660.668990.432520.0566*
O240.997470.983180.358520.0566*
O251.098020.390290.407410.0566*
O260.658721.246480.318700.0566*
N270.162430.516930.604410.0400*
H290.160900.493590.531980.0500*
H300.339930.438700.634880.0500*
H310.136950.710680.623730.0500*
H320.019910.417340.627010.0500*
N280.591710.129780.476460.0400*
H330.622530.061460.455400.0500*
H340.584720.144310.548560.0500*
H350.415160.208170.444850.0500*
H360.776500.233330.457050.0500*
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N27—H29···O25i1.051.882.907167
N27—H30···O26ii1.041.952.979172
N27—H31···O24iii1.061.622.650162
N27—H32···O26iv1.041.902.942174
N28—H33···O23v1.061.622.655164
N28—H34···O26ii1.042.003.007164
N28—H35···O25i1.041.882.904169
N28—H36···O251.051.852.885172
Symmetry codes: (i) x1, y, z; (ii) x, y1, z+1; (iii) x1, y, z+1; (iv) x1, y1, z+1; (v) x, y1, z.
 

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