Crystal structure of bis(µ2- 4-iodopyridine-2,6-dicarboxylato-κ3 O:N:O′)-bis(4-iodopyridine-2,6-dicarboxylato-κ3 O:N:O′)-bis(µ2-1-(4-pyridyl)piperazine-κ2 N:N′)-hexa-aqua-tetra-copper(II), C46H46Cu4I4N10O22
Lv, Benlian; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 957–959; doi:10.1515/ncrs-2021-0166

data_8104634
_publ_section_title
;
 Crystal structure of bis(&#x00B5;2- 4-iodopyridine-2,6-dicarboxylato-\k3
 O:N:O&#x2032;)-bis(4-iodopyridine-2,6-dicarboxylato-\k3
 O:N:O&#x2032;)-bis(&#x00B5;2-1-(4-pyridyl)piperazine-\k2
 N:N&#x2032;)-hexa-aqua-tetra-copper(II), C46H46Cu4I4N10O22
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              957
_journal_page_last               959
_journal_paper_doi               10.1515/ncrs-2021-0166
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C46 H46 Cu4 I4 N10 O22'
_chemical_formula_sum            'C46 H46 Cu4 I4 N10 O22'
_chemical_formula_weight         1852.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 93.853(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6637(2)
_cell_length_b                   18.8249(6)
_cell_length_c                   14.8626(5)
_cell_measurement_reflns_used    7054
_cell_measurement_temperature    291.0(4)
_cell_measurement_theta_max      27.5670
_cell_measurement_theta_min      3.9660
_cell_volume                     2976.82(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      291.0(4)
_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    -30.00  54.00   1.00    4.00    --  -13.49  57.00 -30.00   84
  2  \w    -13.00  41.00   1.00    4.00    --  -13.49  57.00  90.00   54
  3  \w    -83.00   5.00   1.00    4.00    --  -13.49 -38.00 -30.00   88
  4  \w    -11.00  64.00   1.00    4.00    --   14.89  77.00-150.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0450506000
_diffrn_orient_matrix_UB_12      0.0053393000
_diffrn_orient_matrix_UB_13      0.0366718000
_diffrn_orient_matrix_UB_21      -0.0250358000
_diffrn_orient_matrix_UB_22      -0.0293192000
_diffrn_orient_matrix_UB_23      0.0227973000
_diffrn_orient_matrix_UB_31      0.0422816000
_diffrn_orient_matrix_UB_32      -0.0230653000
_diffrn_orient_matrix_UB_33      -0.0205574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17298
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.418
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    2.067
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0212P)^2^+5.5089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4340
_reflns_number_total             5227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0166_suppl.cif
_cod_data_source_block           exp_5222
_cod_original_cell_volume        2976.81(15)
_cod_database_code               8104634
_shelx_estimated_absorpt_t_max   0.435
_shelx_estimated_absorpt_t_min   0.395
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O11(H11A,H11B)
2.b Rotating group:
 O5(H5A,H5B), O10(H10A,H10B)
2.c Ternary CH refined with riding coordinates:
 N2(H2)
2.d Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10C,H10D), C11(H11C,H11D)
2.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C21(H21)
;