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_7711583
_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            'C22 H40 Ag K N2 O8 S4'
_chemical_formula_weight         735.77
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_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                120
_cell_formula_units_Z            6
_cell_length_a                   9.656(2)
_cell_length_b                   9.656(2)
_cell_length_c                   57.87(2)
_cell_measurement_reflns_used    3497
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.498
_cell_measurement_theta_min      2.112
_cell_volume                     4673(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            36217
_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         27.497
_diffrn_reflns_theta_min         2.535
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  0.8732
_exptl_absorpt_correction_T_min  0.8021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
; 
 Flack x determined using 1116 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.024(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.336
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3589
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.351
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+11.1122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.571
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3495
_reflns_number_total             3589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02768b2.cif
_cod_data_source_block           hjw02_Lee
_cod_original_cell_volume        4672(3)
_cod_database_code               7711583
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.880
_shelx_res_checksum              28550