Regulating the coordination geometry of polyhedra in zero-dimensional metal halides for tunable emission.
Zhang, Zhipeng; Liao, Jin-Feng; Xing, Guichuan; Nanoscale 15 (2023) 5241–5248; doi:10.1039/d2nr06975j

data_1568467
_publ_section_title
;
 Regulating the coordination geometry of polyhedra in zero-dimensional
 metal halides for tunable emission.
;
_journal_issue                   11
_journal_name_full               Nanoscale
_journal_page_first              5241
_journal_page_last               5248
_journal_paper_doi               10.1039/d2nr06975j
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'Br4 Pb, 2(C10 H22 N)'
_chemical_formula_sum            'C20 H44 Br4 N2 Pb'
_chemical_formula_weight         839.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-12-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-01-31 deposited with the CCDC.	2023-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.1860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4084(9)
_cell_length_b                   8.4516(4)
_cell_length_c                   18.5924(8)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      59.23
_cell_measurement_theta_min      3.77
_cell_volume                     2714.1(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29854
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.110
_diffrn_reflns_theta_min         2.358
_diffrn_source_current           3.57
_diffrn_source_power             0.249543
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    12.114
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5004
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1592 before and 0.0799 after correction.
The Ratio of minimum to maximum transmission is 0.6658.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00048(7)
_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   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0180P)^2^+17.4331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2936
_reflns_number_total             2978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr06975j2.cif
_cod_data_source_block           aaa
_cod_depositor_comments
'Adding full bibliography for 1568465--1568467.cif.'
_cod_database_code               1568467
_shelx_shelxl_version_number     2014/7
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C13(H13A,
 H13B), C11(H11A,H11B), C12(H12A,H12B)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'