Multi-step structural phase transitions with novel symmetry breaking and inverse symmetry breaking characteristics in a [Ag<sub>4</sub>I<sub>6</sub>]<sup>2-</sup> cluster hybrid crystal.
Zhang, Jin; Yao, Wan-Wan; Sang, Lei; Pan, Xue-Wei; Wang, Xiao-Zu; Liu, Wen-Long; Wang, Lifeng; Ren, Xiao-Ming; Chemical communications (Cambridge, England) 56 (2020) 462–465; doi:10.1039/c9cc08394d

data_7125721
_publ_section_title
;
 Multi-step structural phase transitions with novel symmetry breaking and
 inverse symmetry breaking characteristics in a
 [Ag<sub>4</sub>I<sub>6</sub>]<sup>2-</sup> cluster hybrid crystal.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              462
_journal_page_last               465
_journal_paper_doi               10.1039/c9cc08394d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C18 H38 Ag4 I6 N4'
_chemical_formula_sum            'C18 H38 Ag4 I6 N4'
_chemical_formula_weight         1503.40
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-21
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2019-11-22 deposited with the CCDC.	2019-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1410(9)
_cell_length_b                   15.1410(9)
_cell_length_c                   15.1410(9)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    408
_cell_measurement_theta_max      25.078
_cell_measurement_theta_min      2.349
_cell_volume                     3471.1(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      408
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33119
_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         27.613
_diffrn_reflns_theta_min         2.690
_exptl_absorpt_coefficient_mu    7.575
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0839 before and 0.0624 after correction. The Ratio of minimum to maximum transmission is 0.7606. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.877
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1356
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+11.0148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                756
_reflns_number_total             1356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08394d2.cif
_cod_data_source_block           c135
_cod_original_cell_volume        3471.1(6)
_cod_database_code               7125721
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.582
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C4 = C4-C5
 1.53 with sigma of 0.02
 I1-Ag1 \\sim I1B-Ag1
 with sigma of 0.02
 I1-Ag2 \\sim I1B-Ag2
 with sigma of 0.02
 N1-C1 \\sim N2-C2
 with sigma of 0.02
3. Rigid bond restraints
 N1, C1, C2, N2, C3, C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: I1(0.33333) I1A(0.33333) I1B(0.33333) Ag1(0.33333) Ag2(0.33333)
 H3A(0.33333) H3B(0.33333) C4(0.33333) H4A(0.33333) H4B(0.33333) H5A(0.33333)
 H5B(0.33333) H5C(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
6.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              72656
_olex2_submission_special_instructions 'No special instructions were received'