A lead-free perovskite-like hybrid with above-room-temperature switching of quadratic nonlinear optical properties.
Zhang, Jing; Han, Shiguo; Liu, Xitao; Wu, Zhenyue; Ji, Chengmin; Sun, Zhihua; Luo, Junhua; Chemical communications (Cambridge, England) 54 (2018) 5614–5617; doi:10.1039/c8cc02496k

data_7121528
_publ_section_title
;
 A lead-free perovskite-like hybrid with above-room-temperature switching
 of quadratic nonlinear optical properties.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5614
_journal_page_last               5617
_journal_paper_doi               10.1039/c8cc02496k
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'Cl4 Sb, Cl, C12 H28 N2'
_chemical_formula_sum            'C12 H28 Cl5 N2 Sb'
_chemical_formula_weight         499.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-28 deposited with the CCDC.
2018-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0708(7)
_cell_length_b                   7.9573(5)
_cell_length_c                   20.1605(10)
_cell_measurement_reflns_used    2301
_cell_measurement_temperature    350.00(10)
_cell_measurement_theta_max      22.8910
_cell_measurement_theta_min      4.0320
_cell_volume                     2096.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      350.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -65.00  38.00   1.00   25.25    --   11.39 -38.00  90.00  103
  2  \w     -1.00  42.00   1.00   25.25    --   11.39  57.00 -90.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0222630000
_diffrn_orient_matrix_UB_12      -0.0788264000
_diffrn_orient_matrix_UB_13      0.0078340000
_diffrn_orient_matrix_UB_21      0.0388615000
_diffrn_orient_matrix_UB_22      0.0413337000
_diffrn_orient_matrix_UB_23      0.0183478000
_diffrn_orient_matrix_UB_31      -0.0306364000
_diffrn_orient_matrix_UB_32      -0.0048862000
_diffrn_orient_matrix_UB_33      0.0289813000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7734
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.493
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.947
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2718
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0818P)^2^+3.0427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1547
_reflns_number_total             2718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02496k2.cif
_cod_data_source_block           350K
_cod_depositor_comments
'Adding full bibliography for 7121527--7121528.cif.'
_cod_database_code               7121528
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Sb Cl'
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C6
 with sigma of 0.02
 C7-C8 \\sim C8-C9 \\sim C9-C10 \\sim C10-C11 \\sim C11-C12
 with sigma of 0.02
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H4A(0.5) H4B(0.5) H1C(0.5) H1D(0.5) H2A(0.5)
 H2B(0.5) H5A(0.5) H5B(0.5) H3A(0.5) H3B(0.5) H6A(0.5) H6B(0.5) H9A(0.5)
 H9B(0.5) H7A(0.5) H7B(0.5) H12A(0.5) H12B(0.5) H2C(0.5) H2D(0.5) H11A(0.5)
 H11B(0.5) H10A(0.5) H10B(0.5) H8A(0.5) H8B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C4(H4A,H4B), C1(H1C,H1D), C2(H2A,H2B), C5(H5A,H5B), C3(H3A,H3B),
 C6(H6A,H6B), C9(H9A,H9B), C7(H7A,H7B), C12(H12A,H12B), N2(H2C,H2D), C11(H11A,
 H11B), C10(H10A,H10B), C8(H8A,H8B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.838