Crystal structure of poly[bis{μ2-5-carboxy-4′-methyl-[1,1′-biphenyl]-3-carboxylato-κ2 O:O′}-{μ2-4,4′-bipyridine-κ2N:N′}]cobalt(II), C40H30N2O8Co
Hu, Shao-Qiang; Li, Shi-Hui; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1137–1139; doi:10.1515/ncrs-2020-0205

data_8105401
_publ_section_title
;
 Crystal structure of
 poly[bis{\m2-5-carboxy-4&#x2032;-methyl-[1,1&#x2032;-biphenyl]-3-carboxylato-\k2
 O:O&#x2032;}-{\m2-4,4&#x2032;-bipyridine-\k2N:N&#x2032;}]cobalt(II),
 C40H30N2O8Co
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1137
_journal_page_last               1139
_journal_paper_doi               10.1515/ncrs-2020-0205
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C40 H30 Co N2 O8'
_chemical_formula_sum            'C40 H30 Co N2 O8'
_chemical_formula_weight         725.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                84.534(5)
_cell_angle_beta                 85.582(5)
_cell_angle_gamma                79.413(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8766(6)
_cell_length_b                   11.5473(8)
_cell_length_c                   14.2194(9)
_cell_measurement_reflns_used    2542
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1440
_cell_measurement_theta_min      4.1690
_cell_volume                     1583.90(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -81.00   3.00   1.00   17.00    --  -13.48 -57.00  90.00   84
  2  \w    -40.00  54.00   1.00   17.00    --  -13.48  77.00-150.00   94
  3  \w    -20.00  25.00   1.00   17.00    --  -13.48 -99.00 -30.00   45
  4  \w    -32.00  56.00   1.00   17.00    --  -13.48  38.00 -60.00   88
  5  \w    -83.00   5.00   1.00   17.00    --  -13.48 -38.00 -90.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0123139000
_diffrn_orient_matrix_UB_12      -0.0589562000
_diffrn_orient_matrix_UB_13      -0.0130860000
_diffrn_orient_matrix_UB_21      0.0087632000
_diffrn_orient_matrix_UB_22      -0.0213120000
_diffrn_orient_matrix_UB_23      0.0479963000
_diffrn_orient_matrix_UB_31      -0.0716178000
_diffrn_orient_matrix_UB_32      -0.0013553000
_diffrn_orient_matrix_UB_33      0.0067441000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.1102
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12944
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.32
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         5740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                3354
_reflns_number_total             5740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2020-0205_suppl.cif
_cod_data_source_block           6
_cod_original_cell_volume        1583.90(17)
_cod_database_code               8105401
_chemical_oxdiff_formula         'C H N O CO'
_reflns_odcompleteness_completeness 98.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C40(H40), C39(H39), C37(H37), C36(H36), C3(H3), C5(H5A), C7(H7A), C9(H9),
 C10(H10), C12(H12), C13(H13), C18(H18), C20(H20), C22(H22), C24(H24), C25(H25),
  C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C29(H29A,H29B,H29C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.095
_oxdiff_exptl_absorpt_empirical_full_min 0.476