Crystal structure of poly[di-μ2-aqua)-diaqua-bis(μ6-4,4′,4′′-(benzene-1,3,5-triyltris(oxy))tribenzoato-κ6O1:O2:O3:O3:O5:O6)tricadmium(II)] dihydrate, C54H42Cd3O24
Zhang, Peng; Su, Yan; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 693–695; doi:10.1515/ncrs-2019-0042

data_8105823
_publ_section_title
;
 Crystal structure of
 poly[di-\m2-aqua)-diaqua-bis(\m6-4,4&#x2032;,4&#x2032;&#x2032;-(benzene-1,3,5-triyltris(oxy))tribenzoato-\k6O1:O2:O3:O3:O5:O6)tricadmium(II)]
 dihydrate, C54H42Cd3O24
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              693
_journal_page_last               695
_journal_paper_doi               10.1515/ncrs-2019-0042
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C54 H38 Cd3 O22, 2(H2 O)'
_chemical_formula_sum            'C54 H42 Cd3 O24'
_chemical_formula_weight         1412.07
_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   mixed
_cell_angle_alpha                95.174(5)
_cell_angle_beta                 100.765(6)
_cell_angle_gamma                107.158(6)
_cell_formula_units_Z            1
_cell_length_a                   7.9122(5)
_cell_length_b                   9.0693(6)
_cell_length_c                   18.6637(11)
_cell_measurement_reflns_used    4026
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8620
_cell_measurement_theta_min      3.8330
_cell_volume                     1242.00(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2542
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_details
;
  1 omega   23.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7173   57.0000    0.0000 59

  2 omega  -31.00   39.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7173  -57.0000  -90.0000 70

  3 omega  -51.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7173  -57.0000   60.0000 82

  4 omega   69.00   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7173  178.0000  120.0000 25

  5 omega   -4.00   87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7173   57.0000 -150.0000 91

  6 omega  -21.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6704  -99.0000   90.0000 42

  7 omega   -3.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6704  -99.0000 -180.0000 25

  8 omega   18.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6704   19.0000  -30.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0067611000
_diffrn_orient_matrix_UB_12      -0.0200614000
_diffrn_orient_matrix_UB_13      -0.0367403000
_diffrn_orient_matrix_UB_21      -0.0718304000
_diffrn_orient_matrix_UB_22      0.0291859000
_diffrn_orient_matrix_UB_23      -0.0133826000
_diffrn_orient_matrix_UB_31      0.0637452000
_diffrn_orient_matrix_UB_32      0.0748992000
_diffrn_orient_matrix_UB_33      0.0020784000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10241
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.980
_diffrn_reflns_theta_min         3.132
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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    1.888
_exptl_crystal_description       block
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0255P)^2^+0.6864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4844
_reflns_number_total             5600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0042_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1241.99(15)
_cod_database_code               8105823
_chemical_oxdiff_formula         'C H O N Cd'
_chemical_oxdiff_usercomment     ZH-342
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.718
_reflns_odcompleteness_completeness 99.66
_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 C(H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O12(H12A,H12B)
2.b Rotating group:
 O11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C19(H19), C20(H20), C23(H23), C25(H25), C27(H27)
;
_olex2_submission_special_instructions 'No special instructions were received'