A 1D chiral infinite chain organic metal halide hybrid with excellent SHG switching and moderate spontaneous polarization
Zhuang, Jia-Chang; Tan, Yui-Hui; Fan, Xiao-Wei; Tang, Yun-Zhi; Song, Ning; Zhang, Yi-Hua; Zhang, Hao; Chen, Shao-Peng; New Journal of Chemistry 46 (2022) 7103–7107; doi:10.1039/D2NJ00303A

data_7061367
_publ_section_title
;
 A 1D chiral infinite chain organic metal halide hybrid with excellent SHG
 switching and moderate spontaneous polarization
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7103
_journal_page_last               7107
_journal_paper_doi               10.1039/D2NJ00303A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'Cl5 Sb, 2(C4 H10 N O)'
_chemical_formula_sum            'C8 H20 Cl5 N2 O2 Sb'
_chemical_formula_weight         475.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-06-26
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2022-01-13 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7467(4)
_cell_length_b                   11.3654(5)
_cell_length_c                   17.6409(9)
_cell_measurement_reflns_used    9716
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      27.369
_cell_measurement_theta_min      2.924
_cell_volume                     1753.68(14)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0328
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21133
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.939
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.331
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.6334.
The \l/2 correction factor is Not present.
;
_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    1.800
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.613
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.241
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3074
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      5.708
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0877
_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^)+(0.1981P)^2^+2.3757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2589
_refine_ls_wR_factor_ref         0.2891
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2565
_reflns_number_total             3074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00303a2.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 7061367.cif.'
_cod_database_code               7061367
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.933
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8(2)
 0.2(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 O1-C3 = O2-C6
 1.431 with sigma of 0.001
 O2-C5 = O2-C7 = O1-C2 = O1-C4
 2.344 with sigma of 0.001
 C7-C5 = C4-C2
 2.34 with sigma of 0.001
 C6-C5 = C7-C6 = C3-C2 = C4-C3
 1.485 with sigma of 0.001
 Cl1_$2-H1
 2.271 with sigma of 0.001
 C2-C1 = C8-C7
 1.501 with sigma of 0.001
 Cl4_$1-H2
 2.04 with sigma of 0.001
 N2-C5 = N2-C8 = N1A-C1 = N1A-C4
 1.485 with sigma of 0.001
 N2-C6 = C8-C6 = C3-C1 = N1A-C3
 2.352 with sigma of 0.001
 H2-O2
 0.85 with sigma of 0.001
 H1-Cl1_$2
 2.322 with sigma of 0.001
 H1b-H7b
 2.1 with sigma of 0.01
 H1b-H6
 2.1 with sigma of 0.01
 H3_$3-H1Ab
 2.1 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(N1A) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(N1A) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(C5) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 N2, O2, C7, C6, C5, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N1A, O1, C3, C4, C2, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6.a Everything fixed:
 O1, O2, H2, C8
6.b Riding coordinates:
 O1(H1)
6.c Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
6.d Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C4(H4a,H4b), N1A(H1Aa,H1Ab), C8(H8a,H8b), C7(H7a,
 H7b), C5(H5a,H5b), N2(H2c,H2d)
;
_shelx_res_checksum              20120
_olex2_submission_special_instructions 'No special instructions were received'