Crystal structure of dodecaaqua-bis(μ2-4,4′-bipyridine-κ2 N:N′)-bis(4,4′-((5-carboxylato-1,3-phenylene)bis(oxy))dibenzoato-κ1 O)tricopper(II) - water (1/4), C62H70Cu3N4O32
Deng, Peng; Li, Da; Zhou, Yan; Ling, Zhi-Hong; Li, Yue-Ming; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 499–501; doi:10.1515/ncrs-2018-0493

data_8105760
_publ_section_title
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 Crystal structure of dodecaaqua-bis(\m2-4,4&#x2032;-bipyridine-\k2
 N:N&#x2032;)-bis(4,4&#x2032;-((5-carboxylato-1,3-phenylene)bis(oxy))dibenzoato-\k1
 O)tricopper(II) - water (1/4), C62H70Cu3N4O32
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_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              499
_journal_page_last               501
_journal_paper_doi               10.1515/ncrs-2018-0493
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C62 H62 Cu3 N4 O28, 4(H2 O)'
_chemical_formula_sum            'C62 H70 Cu3 N4 O32'
_chemical_formula_weight         1573.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 102.286(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   44.710(7)
_cell_length_b                   12.8847(17)
_cell_length_c                   11.9901(18)
_cell_measurement_reflns_used    3664
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3153
_cell_measurement_theta_min      2.9572
_cell_volume                     6749.0(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2542
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   48.00   86.25   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642   77.0000  120.0000 51

  2 omega  -12.00   36.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642   77.0000  120.0000 64

  3 omega   35.00   92.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642  178.0000   90.0000 76

  4 omega  -40.00   -7.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642  -77.0000 -180.0000 44

  5 omega   19.00   46.00   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642  -77.0000 -180.0000 36

  6 omega   -1.00   87.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642   57.0000  -90.0000 118

  7 omega  -82.00  -56.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8892  -57.0000  120.0000 34
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0016663000
_diffrn_orient_matrix_UB_12      -0.0039676000
_diffrn_orient_matrix_UB_13      -0.0600645000
_diffrn_orient_matrix_UB_21      0.0160828000
_diffrn_orient_matrix_UB_22      -0.0040374000
_diffrn_orient_matrix_UB_23      0.0071482000
_diffrn_orient_matrix_UB_31      -0.0010618000
_diffrn_orient_matrix_UB_32      -0.0547450000
_diffrn_orient_matrix_UB_33      0.0038386000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.1000
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19105
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.039
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             3252
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         6864
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0959P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1978
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3826
_reflns_number_total             6864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0493_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105760
_chemical_oxdiff_formula         'C H O N Cu'
_chemical_oxdiff_usercomment     hjy12031268
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.734
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O10-H10B
 0.85 with sigma of 0.01
 O16-H16B
 0.85 with sigma of 0.01
 H14A_$1-H14A
 2.21 with sigma of 0.005
3.a Free rotating group:
 O10(H10A), O16(H16A)
3.b Rotating group:
 O1(H1A,H1B), O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B),
 O15(H15A,H15B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C16(H16), C17(H17), C20(H20), C21(H21), C23(H23), C24(H24), C27(H27),
  C29(H29), C31(H31)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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