The crystal structure of poly[bis(4-hydroxybenzoato-κO)-(μ2-4,4′-bipyridine-κ2 N:N′)copper(II)] hydrate, C24H20N2O7Cu
He, Haiyan; Li, Yuyang; Yang, Qiucheng; Li, Lei; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 621–623; doi:10.1515/ncrs-2017-0377

data_8106236
_publ_section_title
;
 The crystal structure of
 poly[bis(4-hydroxybenzoato-\kO)-(\m2-4,4&#x2032;-bipyridine-\k2
 N:N&#x2032;)copper(II)] hydrate, C24H20N2O7Cu
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              621
_journal_page_last               623
_journal_paper_doi               10.1515/ncrs-2017-0377
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         '0.5(C48 H36 Cu2 N4 O12), H2 O'
_chemical_formula_sum            'C24 H20 Cu N2 O7'
_chemical_formula_weight         511.96
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.163(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6241(4)
_cell_length_b                   10.4639(2)
_cell_length_c                   10.7024(2)
_cell_measurement_reflns_used    3090
_cell_measurement_temperature    293
_cell_measurement_theta_max      70.6350
_cell_measurement_theta_min      4.5280
_cell_volume                     2184.98(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -22.00  69.00   1.00    1.00    --    0.00  57.00 -90.00   91
  2  \w    -53.00   5.00   1.00    1.00    --    0.00 117.00 -38.00   58
  3  \w      1.00  98.00   1.00    1.00    --   54.00 -99.00 120.00   97
  4  \w     95.00 120.00   1.00    1.00    --   54.00 163.00 110.00   25
  5  \w     32.00 115.00   1.00    1.00    --   54.00  57.00  90.00   83
  6  \w     36.00  90.00   1.00    1.00    --   54.00  57.00-180.00   54
  7  \w     17.00  75.00   1.00    1.00    --   54.00 -57.00-150.00   58
  8  \w    100.00 132.00   1.00    1.00    --  108.00 -63.00-120.00   32
  9  \w     54.00  89.00   1.00    1.00    --  108.00 -63.00-120.00   35
 10  \w     59.00 145.00   1.00    1.00    --  108.00 -91.00 -30.00   86
 11  \w     50.00 135.00   1.00    1.00    --  108.00 -38.00 120.00   85
 12  \w     35.00 115.00   1.00    1.00    --  108.00-111.00 150.00   80
 13  \w     88.00 164.00   1.00    1.00    --  108.00  63.00  90.00   76
 14  \w     59.00 158.00   1.00    1.00    --  108.00 -12.00-120.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0113441000
_diffrn_orient_matrix_UB_12      -0.1316846000
_diffrn_orient_matrix_UB_13      0.0587205000
_diffrn_orient_matrix_UB_21      0.0773800000
_diffrn_orient_matrix_UB_22      -0.0275881000
_diffrn_orient_matrix_UB_23      0.0060367000
_diffrn_orient_matrix_UB_31      0.0107925000
_diffrn_orient_matrix_UB_32      0.0597078000
_diffrn_orient_matrix_UB_33      0.1322579000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3864
_diffrn_reflns_theta_full        67.06
_diffrn_reflns_theta_max         67.06
_diffrn_reflns_theta_min         4.53
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.852
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0046(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0461P)^2^+2.2428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                1878
_reflns_number_total             1956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0377_suppl.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        2184.99(8)
_cod_database_code               8106236
_chemical_oxdiff_formula         'C H N O Cu'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C2(H2A), C3(H3), C9(H9), C12(H12)
2.b Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_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 1.204
_oxdiff_exptl_absorpt_empirical_full_min '0.792 '