Crystal structure of catena-poly[(μ3-2-carboxy-4-(3-carboxy-5-carboxylatophenoxy)benzoato-κ3O:O′:O′′)-bis(μ2-4,4′-bis(pyrid-4-yl)biphenyl-k1 N)copper(II)], C60H40N4O9Cu
Li, Shi-Hui; Tang, Qian-Qian; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1285–1287; doi:10.1515/ncrs-2020-0266

data_8105445
_publ_section_title
;
 Crystal structure of
 catena-poly[(\m3-2-carboxy-4-(3-carboxy-5-carboxylatophenoxy)benzoato-\k3O:O&#x2032;:O&#x2032;&#x2032;)-bis(\m2-4,4&#x2032;-bis(pyrid-4-yl)biphenyl-k1
 N)copper(II)], C60H40N4O9Cu
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1285
_journal_page_last               1287
_journal_paper_doi               10.1515/ncrs-2020-0266
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C60 H40 Cu N4 O9'
_chemical_formula_sum            'C60 H40 Cu N4 O9'
_chemical_formula_weight         1024.50
_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
_audit_contact_author_name
;
;
_audit_creation_date             2020-05-27
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_cell_angle_alpha                97.162(5)
_cell_angle_beta                 90.953(6)
_cell_angle_gamma                107.788(7)
_cell_formula_units_Z            2
_cell_length_a                   9.6569(8)
_cell_length_b                   10.3941(7)
_cell_length_c                   24.9421(16)
_cell_measurement_reflns_used    5752
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4720
_cell_measurement_theta_min      3.6610
_cell_volume                     2361.3(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -40.00  54.00   1.00    9.60    --  -13.48  77.00  60.00   94
  2  \w    -40.00  54.00   1.00    9.60    --  -13.48  77.00 120.00   94
  3  \w    -12.00  82.00   1.00    9.60    --   14.41  77.00 -30.00   94
  4  \w    -12.00  82.00   1.00    9.60    --   14.41  77.00   0.00   94
  5  \w    -12.00  82.00   1.00    9.60    --   14.41  77.00-180.00   94
  6  \w     12.00  82.00   1.00    9.60    --   14.41  77.00-150.00   70
;
_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      -0.0108890000
_diffrn_orient_matrix_UB_12      0.0349703000
_diffrn_orient_matrix_UB_13      0.0250722000
_diffrn_orient_matrix_UB_21      0.0690649000
_diffrn_orient_matrix_UB_22      0.0004484000
_diffrn_orient_matrix_UB_23      0.0103128000
_diffrn_orient_matrix_UB_31      0.0328893000
_diffrn_orient_matrix_UB_32      0.0633262000
_diffrn_orient_matrix_UB_33      -0.0094486000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.1136
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25258
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49211
_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            green
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         8764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                5613
_reflns_number_total             8764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2020-0266_suppl.cif
_cod_data_source_block           666
_cod_database_code               8105445
_chemical_oxdiff_formula         'C H N O CU'
_reflns_odcompleteness_completeness 99.77
_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 O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33),
 C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44),
  C47(H47), C49(H49), C51(H51), C54(H54), C55(H55), C58(H58)
2.b Idealised tetrahedral OH refined as rotating group:
 O3(H3), O9(H9)
;