Supramolecular assembly and structural transformation of d10-metal complexes containing (aza-15-crown-5)dithiocarbamate
Tzeng, Biing-Chiau; Wu, Chung-Lun; Hung, Jun-Wei; Chien, Su-Ying; Lee, Gene-Hsiang; Dalton Transactions  (2022) –; doi:10.1039/D2DT02768B

data_7711580
_publ_section_title
;
 Supramolecular assembly and structural transformation of d10-metal
 complexes containing (aza-15-crown-5)dithiocarbamate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02768B
_journal_year                    2022
_chemical_formula_sum            'C52 H92 Cu4 N8 O16 S8'
_chemical_formula_weight         1595.97
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-08-06 deposited with the CCDC.	2022-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.5073(4)
_cell_length_b                   19.5073(4)
_cell_length_c                   8.9948(2)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.49
_cell_volume                     3422.83(13)
_computing_cell_refinement       'Bruker SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            38501
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.493
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_T_max  0.7677
_exptl_absorpt_correction_T_min  0.6849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       columnar
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
; 
 Flack x determined using 2194 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.007(3)
_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     200
_refine_ls_number_reflns         5003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+0.3255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0417
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4840
_reflns_number_total             5003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02768b2.cif
_cod_data_source_block           ic21234
_cod_original_cell_volume        3422.83(16)
_cod_database_code               7711580
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.842
_shelx_res_checksum              59341