Crystal structure of poly[diaqua-(μ 2-2,5-dihydroxyterephthalato-κ2 O:O′)(μ 2-bis(4-pyridylformyl)piperazine-κ2 N:N′)cadmium(II)] dihydrate, C24H28CdN4O12
Lv, Benlian; Ren, Yunli; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 961–963; doi:10.1515/ncrs-2021-0167

data_8104635
_publ_section_title
;
 Crystal structure of poly[diaqua-(\m 2-2,5-dihydroxyterephthalato-\k2
 O:O&#x2032;)(\m 2-bis(4-pyridylformyl)piperazine-\k2
 N:N&#x2032;)cadmium(II)] dihydrate, C24H28CdN4O12
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              961
_journal_page_last               963
_journal_paper_doi               10.1515/ncrs-2021-0167
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C24 H24 Cd N4 O10, 2(H2 O)'
_chemical_formula_sum            'C24 H28 Cd N4 O12'
_chemical_formula_weight         676.90
_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                 102.810(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8592(4)
_cell_length_b                   8.3925(3)
_cell_length_c                   13.9503(5)
_cell_measurement_reflns_used    8672
_cell_measurement_temperature    291.19(10)
_cell_measurement_theta_max      26.6080
_cell_measurement_theta_min      3.8600
_cell_volume                     1353.89(8)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.19(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -20.00  29.00   1.00    5.00    --   -9.62 -99.00-120.00   49
  2  \w    -19.00  82.00   1.00    5.00    --   10.64  19.00  60.00  101
  3  \w     -6.00  78.00   1.00    5.00    --   10.64  57.00-150.00   84
  4  \w    -20.00  50.00   1.00    5.00    --   10.64 -99.00-120.00   70
  5  \w    -61.00  40.00   1.00    5.00    --   10.64 -19.00  30.00  101
  6  \w     -6.00  78.00   1.00    5.00    --   10.64  57.00 120.00   84
  7  \w    -20.00  50.00   1.00    5.00    --   10.64 -99.00 -30.00   70
  8  \w    -20.00   5.00   1.00    5.00    --   10.64 -99.00  30.00   25
;
_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      0.0591050000
_diffrn_orient_matrix_UB_12      0.0220822000
_diffrn_orient_matrix_UB_13      0.0086051000
_diffrn_orient_matrix_UB_21      -0.0067013000
_diffrn_orient_matrix_UB_22      0.0184317000
_diffrn_orient_matrix_UB_23      -0.0505807000
_diffrn_orient_matrix_UB_31      -0.0148444000
_diffrn_orient_matrix_UB_32      0.0795072000
_diffrn_orient_matrix_UB_33      0.0093214000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15330
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.523
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46149
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+1.3498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2117
_reflns_number_total             2347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0167_suppl.cif
_cod_data_source_block           91226
_cod_database_code               8104635
_chemical_oxdiff_formula         'Cd C N O H'
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.773
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B)
2.b Rotating group:
 O4(H4A,H4B)
2.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B)
2.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C6(H6), C3(H3A), C8(H8)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;