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_7125720
_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         '2(C9 H19 Ag2 I3 N2)'
_chemical_formula_sum            'C18 H38 Ag4 I6 N4'
_chemical_formula_weight         1503.40
_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     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                 90.269(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0205(8)
_cell_length_b                   15.0458(10)
_cell_length_c                   15.0407(10)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    323(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.35
_cell_volume                     3399.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      323.15
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker 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  0.0596
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28919
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.356
_exptl_absorpt_coefficient_mu    7.735
_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
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.938
_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         1.566
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       21308(500)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5862
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1774
_refine_ls_R_factor_gt           0.1746
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+150.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2956
_refine_ls_wR_factor_ref         0.2958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5133
_reflns_number_total             5862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08394d2.cif
_cod_data_source_block           p2_a
_cod_database_code               7125720
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.698
_shelx_estimated_absorpt_t_min   0.577
_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
 C1-C2 = C3-C4 = C5-C6 = C7-C8 = C9-C10 = C11-C12
 1.53 with sigma of 0.01
 N1-C1 = N1-C3 = N1-C5 = N2-C2 = N2-C4 = N2-C6 = C13-N2 = C16-N4
 1.5 with sigma of 0.01
 N3-C7 = N3-C9 = N3-C11 = N4-C8 = N4-C10 = N4-C12
 1.5 with sigma of 0.01
 C13-C14 = C14-C15 = C16-C17 = C17-C18
 1.55 with sigma of 0.01
 N1-N2 = N3-N4
 2.58 with sigma of 0.01
 N1-C2 = N1-C4 = N1-C6 = N2-C3 = N2-C5 = N2-C1
 2.45 with sigma of 0.01
 N4-C9 = N4-C7 = N4-C11 = N3-C8 = N3-C10 = N3-C12
 2.45 with sigma of 0.01
 C1-C3 = C3-C5 = C5-C1 = C2-C4 = C4-C6 = C6-C2
 2.42 with sigma of 0.01
 C7-C9 = C9-C11 = C11-C7 = C8-C10 = C10-C12 = C12-C8
 2.42 with sigma of 0.01
 N2-C14 = C13-C15 = N4-C17 = C16-C18
 2.42 with sigma of 0.01
3. Rigid bond restraints
 N1, N2, C1, C2, C3, C4, C5, C6, C13, C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, N4, C7, C8, C9, C10, C11, C12, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C13
\\sim C14 \\sim C15: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
N3 \\sim N4 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C16
\\sim C17 \\sim C18: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
5.a Riding coordinates:
 C15(H15A,H15B,H15C), C17(H17A,H17B)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C13(H13A,H13B), C14(H14A,H14B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C16(H16A,H16B)
5.c Me refined with riding coordinates:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              14687
_olex2_submission_special_instructions 'No special instructions were received'