Bulk Assembly of Multicomponent Zero-Dimensional Metal Halides with Dual Emission
Zhou, Chenkun; Lee, Sujin; Lin, Haoran; Neu, Jennifer; Chaaban, Maya; Xu, Liang-Jin; Arcidiacono, Ashley; He, Qingquan; Worku, Michael; Ledbetter, Logan; Lin, Xinsong; Schlueter, John A.; Siegrist, Theo; Ma, Biwu; ACS Materials Letters  (2020) 376–380; doi:10.1021/acsmaterialslett.0c00011

data_4517499
_publ_section_title
;
 Bulk Assembly of Multicomponent Zero-Dimensional Metal Halides with Dual
 Emission
;
_journal_name_full               'ACS Materials Letters'
_journal_page_first              376
_journal_page_last               380
_journal_paper_doi               10.1021/acsmaterialslett.0c00011
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C81 Cl21 N9 Pb3 Sb2'
_chemical_formula_sum            'C81 Cl21 N9 Pb3 Sb2'
_chemical_formula_weight         2708.56
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 119.955(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.7980(5)
_cell_length_b                   30.4525(7)
_cell_length_c                   14.7929(5)
_cell_measurement_reflns_used    17632
_cell_measurement_temperature    119
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     5775.7(4)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      119
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            72657
_diffrn_reflns_theta_full        25.058
_diffrn_reflns_theta_max         28.475
_diffrn_reflns_theta_min         2.754
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.343
_exptl_absorpt_correction_T_max  1.546
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
 Gaussian Integration (Busing and Levy, 1957) 
;
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.213
_refine_diff_density_max         4.46
_refine_diff_density_min         -3.18
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 3899 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.496(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0810
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         8814
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.1856
_refine_ls_R_factor_gt           0.1084
_refine_ls_shift/su_max          0.0020903
_refine_ls_shift/su_mean         0.0002093
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 913. 773. 642. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2132
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.1750
_reflns_limit_h_max              16
_reflns_limit_h_min              -19
_reflns_limit_k_max              40
_reflns_limit_k_min              -40
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                11562
_reflns_number_total             26140
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.17
_oxford_diffrn_Wilson_scale      2.43
_oxford_refine_ls_r_factor_ref   0.0928
_oxford_refine_ls_scale          1.103(4)
_oxford_reflns_number_all        25414
_cod_data_source_file            tz0c00011_si_002.cif
_cod_data_source_block           SbPyPbCl_09182019
_cod_depositor_comments          'Adding full bibliography for 4517499.cif.'
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               4517499
_oxford_refine_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_hooft_y                  0.505(7)
_oxford_bijvoet_difference       0.496(5)