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_7708071
_publ_section_title
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 Two In-based organic--inorganic hybrid compounds with reversible phase
 transition derived from the order--disorder changes of cations or anions
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01935J
_journal_year                    2021
_chemical_formula_moiety         'Br5 H2 In O, C16 H24 N2'
_chemical_formula_sum            'C16 H24 Br5 In N2 O'
_chemical_formula_weight         774.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.910(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.912(8)
_cell_length_b                   8.556(7)
_cell_length_c                   14.164(11)
_cell_measurement_reflns_used    1519
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.84
_cell_volume                     1235.3(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1535
_diffrn_reflns_av_unetI/netI     0.1707
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5950
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.835
_exptl_absorpt_coefficient_mu    9.051
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.0825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1603 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.1106.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.025
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.272
_refine_ls_extinction_coef       0.0117(6)
_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   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2327
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0921
_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^)+(0.1423P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2229
_refine_ls_wR_factor_ref         0.2602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1307
_reflns_number_total             2327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01935j2.cif
_cod_data_source_block           ee
_cod_database_code               7708071
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C6-C5
 1.38 with sigma of 0.02
3. Rigid bond restraints
 C4, C5, C5, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C7 \\sim C4 \\sim C2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C16) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) H2A(0.5) H2C(0.5) H2B(0.5) H1A(0.5) H1B(0.5)
 H1C(0.5) C11(0.5) C16(0.5) H16(0.5) C15(0.5) H15(0.5) C14(0.5) H14(0.5)
 C13(0.5) H13(0.5) C12(0.5) H12(0.5) C8(0.5) H8(0.5) C3(0.5) C7(0.5) H7(0.5)
 C10(0.5) H10A(0.5) H10B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C2(0.5) H2D(0.5)
 H2E(0.5) H4(0.5) H6(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C2(H2D,H2E), C1A(H1AA,H1AB)
6.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C14(H14), C13(H13), C12(H12), C8(H8), C5(H5), C7(H7),
 C4(H4), C6(H6)
6.d Fitted hexagon refined as free rotating group:
 C11(C16,C15,C14,C13,C12)
6.e Idealised Me refined as rotating group:
 N2(H2A,H2C,H2B), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              88023
_shelx_hkl_checksum              24366
_olex2_submission_special_instructions 'No special instructions were received'