Two low-dimensional metal halides: ionothermal synthesis, photoluminescence, and nonlinear optical properties
Deng, Yuandan; Dong, Xuehua; Yang, Meng; Zeng, Hongmei; Zou, Guohong; Lin, Zhien; Dalton Transactions  (2019) –; doi:10.1039/C9DT04102H

data_7701865
_publ_section_title
;
 Two low-dimensional metal halides: ionothermal synthesis,
 photoluminescence, and nonlinear optical properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04102H
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Br3 Pb, C6 H11 N2'
_chemical_formula_sum            'C6 H11 Br3 N2 Pb'
_chemical_formula_weight         558.09
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-08 deposited with the CCDC.	2019-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.19366(13)
_cell_length_b                   9.78266(16)
_cell_length_c                   15.4593(4)
_cell_measurement_reflns_used    2359
_cell_measurement_temperature    295.11(10)
_cell_measurement_theta_max      72.4750
_cell_measurement_theta_min      5.3350
_cell_volume                     1239.15(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.11(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.001
_diffrn_measured_fraction_theta_max 1.000
_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   -106.00 -18.00   1.00    8.00    --  -36.42 -38.00   0.00   88
  2  \w   -104.00 -20.00   1.00    8.00    --  -36.42 -57.00-120.00   84
  3  \w      1.00  75.00   1.00    8.00    --   36.42 -99.00-150.00   74
  4  \w    -31.00  53.00   1.00    8.00    --   36.42 -57.00 -60.00   84
  5  \w     39.00 130.00   1.00   25.00    --  108.71 -30.00 120.00   91
  6  \w     39.00 115.00   1.00   25.00    --  108.71-111.00   0.00   76
  7  \w     68.00  94.00   1.00   25.00    --  108.71 -94.00-180.00   26
  8  \w     47.00 109.00   1.00   25.00    --  108.71 -94.00-120.00   62
  9  \w     72.00 159.00   1.00   25.00    --  108.71  15.00 150.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0274132000
_diffrn_orient_matrix_UB_12      0.1447275000
_diffrn_orient_matrix_UB_13      0.0365906000
_diffrn_orient_matrix_UB_21      0.0118663000
_diffrn_orient_matrix_UB_22      -0.0569369000
_diffrn_orient_matrix_UB_23      0.0926989000
_diffrn_orient_matrix_UB_31      0.1855341000
_diffrn_orient_matrix_UB_32      0.0251640000
_diffrn_orient_matrix_UB_33      -0.0005082000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 1.001
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3634
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.034
_diffrn_reflns_theta_max         67.034
_diffrn_reflns_theta_min         5.351
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    37.475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.991
_exptl_crystal_description       needle
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.786
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.345
_refine_ls_abs_structure_details
;
 Flack x determined using 696 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.069(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0968P)^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         0.1351
_reflns_Friedel_coverage         0.573
_reflns_Friedel_fraction_full    0.810
_reflns_Friedel_fraction_max     0.810
_reflns_number_gt                1984
_reflns_number_total             2039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04102h2.cif
_cod_data_source_block           yd1-5-9
_cod_database_code               7701865
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.117
_shelx_estimated_absorpt_t_min   0.021
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C2(H2)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              39900
_olex2_date_sample_data_collection 2018-11-20
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.737
_oxdiff_exptl_absorpt_empirical_full_min 0.669