Investigation of four Cd(ii) sulfonate complexes: crystal structure, Hirshfeld surface analysis, thermogravimetric and spectroscopic properties
Wang, Xueyuan; Carrillo-Aravena, Eduardo; Wu, Yuandong; Mei, Dajiang; Wen, Shaoguo; Doert, Thomas; CrystEngComm 25 (2023) 5673–5681; doi:10.1039/D3CE00792H

data_7247425
_publ_section_title
;
 Investigation of four Cd(ii) sulfonate complexes: crystal structure,
 Hirshfeld surface analysis, thermogravimetric and spectroscopic
 properties
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              5673
_journal_page_last               5681
_journal_paper_doi               10.1039/D3CE00792H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_structural
(Cd2((C5H4N)2)3(H2O)6)(C6H7NO3S)2(NO3)2(C5H4N)2(H2O)
_chemical_formula_sum            'C62 H68 Cd2 N14 O20 S2'
_chemical_formula_weight         1618.22
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
'SHELXL-2016/6 & CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
;
_audit_update_record
;
2023-07-17 deposited with the CCDC.	2023-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.423(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3640(1)
_cell_length_b                   23.3599(3)
_cell_length_c                   19.2032(3)
_cell_measurement_reflns_used    33243
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      31.6840
_cell_measurement_theta_min      2.0420
_cell_volume                     3297.49(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'OLEX2 v1.3 (Dolomanov et. al., 2009)'
_computing_publication_material  'DIAMOND v4.6.8'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_detector_type            'Eiger2 1M'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.895
_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     -5.00  94.00   0.30   26.00    --   16.64  38.00 -60.00  330
  2  \w     -5.00  86.20   0.30   26.00    --   16.64  57.00  30.00  304
  3  \w    -16.00  81.20   0.30   26.00    --   16.64  77.00-180.00  324
  4  \w     24.00  49.80   0.30   26.00    --   16.64 -99.00 150.00   86
  5  \w     11.00  55.10   0.30   26.00    --   16.64 -99.00  90.00  147
  6  \w     57.00  85.20   0.30   26.00    --   16.64  77.00-150.00   94
  7  \w    -87.00 -16.80   0.30   26.00    --  -16.79 -57.00  90.00  234
  8  \w    -87.00  15.00   0.30   26.00    --  -16.79 -77.00-120.00  340
  9  \w    -83.00 -57.20   0.30   26.00    --  -16.79-178.00-150.00   86
 10  \w     -3.00  25.20   0.30   26.00    --  -16.79 -19.00 120.00   94
 11  \w    -81.00  -6.00   0.30   26.00    --  -16.79 -19.00 120.00  250
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Eiger2 1M'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0821418000
_diffrn_orient_matrix_UB_12      0.0124420000
_diffrn_orient_matrix_UB_13      0.0140086000
_diffrn_orient_matrix_UB_21      -0.0395159000
_diffrn_orient_matrix_UB_22      0.0276159000
_diffrn_orient_matrix_UB_23      -0.0035574000
_diffrn_orient_matrix_UB_31      -0.0316337000
_diffrn_orient_matrix_UB_32      -0.0022232000
_diffrn_orient_matrix_UB_33      0.0340556000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23771
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.732
_diffrn_reflns_theta_min         1.744
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.073
_refine_diff_density_max         1.246
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         23771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21832
_reflns_number_total             23771
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.6468\% 
around [0.00 1.00 -0.02] (reciprocal) or [0.00 1.00 -0.02] (direct)
;
_cod_data_source_file            d3ce00792h2.cif
_cod_data_source_block           R127_K9
_cod_depositor_comments
'Adding full bibliography for 7247422--7247425.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7247425
_shelx_shelxl_version_number     2016/6
_cell_oxdiff_measurement_reflns_used 30056
_cell_oxdiff_volume              3297.53(8)
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.944
_oxdiff_exptl_absorpt_empirical_full_min 0.614
_oxdiff_exptl_absorpt_empirical_full_max 1.581
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous
_shelx_res_checksum              57055