Crystal structure of 4,4′-bis(pyridin-1-ium-4-yl)biphenyl poly[bis(μ2-4,4′-bis(pyrid-4-yl)biphenyl-K2 N:N′)-tetrakis(μ4-4′-methyl-[1,1′-biphenyl]-3,5-dicarboxylato-K4 O,O′:O′′:O′′′)-bis[[μ2-1,1′-biphenyl]-3-carboxyl-5-carboxylato-K2 O:O′]tetracobalt(II)]— [1,1′-biphenyl]-3,5-dicarboxylic acid (1/2), C93H68N3O16Co2
Tang, Qian-Qian; Li, Shi-Hui; Cheng, Zhan-Quan; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1209–1212; doi:10.1515/ncrs-2020-0255

data_8105423
_publ_section_title
;
 Crystal structure of 4,4&#x2032;-bis(pyridin-1-ium-4-yl)biphenyl
 poly[bis(\m2-4,4&#x2032;-bis(pyrid-4-yl)biphenyl-K2
 N:N&#x2032;)-tetrakis(\m4-4&#x2032;-methyl-[1,1&#x2032;-biphenyl]-3,5-dicarboxylato-K4
 O,O&#x2032;:O&#x2032;&#x2032;:O&#x2032;&#x2032;&#x2032;)-bis[[\m2-1,1&#x2032;-biphenyl]-3-carboxyl-5-carboxylato-K2
 O:O&#x2032;]tetracobalt(II)]--- [1,1&#x2032;-biphenyl]-3,5-dicarboxylic
 acid (1/2), C93H68N3O16Co2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1209
_journal_page_last               1212
_journal_paper_doi               10.1515/ncrs-2020-0255
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C67 H47 Co2 N2 O12, C11 H9 N, C15 H12 O4'
_chemical_formula_sum            'C93 H68 Co2 N3 O16'
_chemical_formula_weight         1601.36
_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                66.036(4)
_cell_angle_beta                 87.374(4)
_cell_angle_gamma                85.610(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9281(4)
_cell_length_b                   19.1304(8)
_cell_length_c                   22.0724(10)
_cell_measurement_reflns_used    11970
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0410
_cell_measurement_theta_min      3.7020
_cell_volume                     3819.1(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -30.00  54.00   1.00   40.00    --  -13.48  57.00   0.00   84
  2  \w    -30.00  54.00   1.00   40.00    --  -13.48  57.00  30.00   84
  3  \w    -83.00   5.00   1.00   40.00    --  -13.48 -38.00-150.00   88
  4  \w    -20.00  25.00   1.00   40.00    --  -13.48 -99.00   0.00   45
  5  \w     -2.00  82.00   1.00   40.00    --   14.41  57.00-120.00   84
  6  \w     -2.00  82.00   1.00   40.00    --   14.41  57.00 150.00   84
  7  \w    -40.00  26.00   1.00   40.00    --  -13.48  77.00-180.00   66
;
_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      -0.0023565000
_diffrn_orient_matrix_UB_12      0.0015339000
_diffrn_orient_matrix_UB_13      0.0316058000
_diffrn_orient_matrix_UB_21      -0.0050670000
_diffrn_orient_matrix_UB_22      0.0406263000
_diffrn_orient_matrix_UB_23      -0.0154172000
_diffrn_orient_matrix_UB_31      -0.0714451000
_diffrn_orient_matrix_UB_32      -0.0003436000
_diffrn_orient_matrix_UB_33      0.0006211000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41860
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53560
_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    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1658
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         14116
_refine_ls_number_restraints     2112
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+1.1153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                10371
_reflns_number_total             14116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2020-0255_suppl.cif
_cod_data_source_block           3
_cod_database_code               8105423
_chemical_oxdiff_formula         'c h n o co'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8A), C10(H10), C11(H11),
 C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C25(H25), C27(H27), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35),
 C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C47(H47), C48(H48),
  C51(H51), C53(H53), C55(H55), C57(H57), C58(H58), C60(H60), C61(H61),
 C66(H66), C68(H68), C70(H70), C72(H72), C73(H73), C75(H75), C76(H76), C81(H81),
  C83(H83), C85(H85), C87(H87), C88(H88), C90(H90), C91(H91)
3.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C62(H62A,H62B,H62C), C78(H78A,H78B,H78C), C93(H93A,H93B,
 H93C)
3.c Idealised tetrahedral OH refined as rotating group:
 O8(H8), O14(H14A), O15(H15)
;
_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 2.716
_oxdiff_exptl_absorpt_empirical_full_min 0.456