Two In-based organic‒inorganic hybrid compounds with reversible phase transition derived from the order‒disorder changes of cations or anions
Zhang, Yin-Qiang; Xu, Guan-Cheng; Li, Min; Dalton Transactions  (2021) –; doi:10.1039/D1DT01935J

data_7708069
_publ_section_title
;
 Two In-based organic--inorganic hybrid compounds with reversible phase
 transition derived from the order--disorder changes of cations or anions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01935J
_journal_year                    2021
_chemical_formula_moiety         'Cl4 In, C12 H28 N'
_chemical_formula_sum            'C12 H28 Cl4 In N'
_chemical_formula_weight         442.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-04-10 deposited with the CCDC.	2021-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.299(4)
_cell_length_b                   16.580(5)
_cell_length_c                   17.771(5)
_cell_measurement_reflns_used    788
_cell_measurement_temperature    380
_cell_measurement_theta_max      14.466
_cell_measurement_theta_min      2.203
_cell_volume                     4213(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      380
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1194
_diffrn_reflns_av_unetI/netI     0.1209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13781
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.202
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1711 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.7572.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3859
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.2182
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0692P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1163
_reflns_number_total             3859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01935j2.cif
_cod_data_source_block           c
_cod_database_code               7708069
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.830
_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
 In1-Cl4B \\sim In1-Cl4A
 with sigma of 0.02
 In1-Cl1B \\sim In1-Cl1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl4A \\sim Cl4B: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Cl1B \\sim Cl1A: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Cl3A \\sim Cl3B: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
4. Rigid body (RIGU) restrains
 C12, N1, C10, C7, C4, C1, C11, C8, C5, C2, C9, C6, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl4A, Cl4B, In1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 In1, Cl2, Cl3B, Cl1B, Cl4B, Cl4A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cl4B)=1-FVAR(1)
 Sof(Cl4A)=FVAR(1)
 Sof(Cl3B)=1-FVAR(2)
 Sof(Cl3A)=FVAR(2)
 Sof(Cl1B)=1-FVAR(3)
 Sof(Cl1A)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C7(H7A,H7B), C4(H4A,H4B), C1(H1A,H1B), C11(H11A,H11B), C2(H2A,
 H2B), C8(H8A,H8B), C5(H5A,H5B)
6.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              7078
_shelx_hkl_checksum              9853
_olex2_submission_special_instructions 'No special instructions were received'