Insight into systematic formation of hexafluorosilicate during crystallization via self-assembly in a glass vessel
Kim, Dongwon; Han, Jihun; Jung, Ok-Sang; Lee, Young-A.; RSC Advances 12 (2022) 25118–25122; doi:10.1039/D2RA04270C

data_7245441
_publ_section_title
;
 Insight into systematic formation of hexafluorosilicate during
 crystallization via self-assembly in a glass vessel
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              25118
_journal_page_last               25122
_journal_paper_doi               10.1039/D2RA04270C
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C216 H168 Cu3 F18 N24 O36 Si3'
_chemical_formula_weight         4292.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-06-21 deposited with the CCDC.	2022-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.69(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   38.961(8)
_cell_length_b                   21.921(4)
_cell_length_c                   23.987(5)
_cell_measurement_reflns_used    140893
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      33.974
_cell_measurement_theta_min      0.435
_cell_volume                     18304(8)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_refinement  SHELXL
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.760
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.1051
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60235
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        27.129
_diffrn_reflns_theta_max         27.150
_diffrn_reflns_theta_min         1.206
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.779
_exptl_crystal_description       block
_exptl_crystal_F_000             4422
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.020
_refine_ls_abs_structure_details
;
 Flack x determined using 4602 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.786
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1312
_refine_ls_number_reflns         32740
_refine_ls_number_restraints     1567
_refine_ls_restrained_S_all      0.787
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0421P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                13318
_reflns_number_total             32740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra04270c2.cif
_cod_data_source_block           CuSiF6_L1
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7245441
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              50888
_shelx_fab_checksum              49219