Solution and Solid-State Characterization of PbSe Precursors
Vartak, Prathamesh B.; Wang, Zhongyong; Groy, Thomas L.; Trovitch, Ryan J.; Wang, Robert Y.; ACS Omega  (2020) –; doi:10.1021/acsomega.9b03715

data_4517354
_publ_section_title
;
 Solution and Solid-State Characterization of PbSe Precursors
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.9b03715
_journal_year                    2020
_chemical_formula_moiety         'C22 H20 N2 Pb Se2'
_chemical_formula_sum            'C22 H20 N2 Pb Se2'
_chemical_formula_weight         677.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 93.8688(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.4824(2)
_cell_length_b                   9.0496(3)
_cell_length_c                   21.3585(8)
_cell_measurement_reflns_used    6541
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      25.3399
_cell_measurement_theta_min      2.4451
_cell_volume                     1057.26(7)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2014)'
_computing_data_collection       'Bruker Instrument Service v2015.5.1.3'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL XT-2014/4'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX Diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8938
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.91
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    11.430
_exptl_absorpt_correction_T_max  0.35
_exptl_absorpt_correction_T_min  0.21
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.479
_refine_diff_density_min         -0.582
_refine_ls_abs_structure_details
;
H. D. Flack (1983). "On Enantiomorph-Polarity Estimation". 
Acta Crystallogr. A39: 876-881.
;
_refine_ls_abs_structure_Flack   -0.032(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3871
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0315P)^2^+1.7019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                3734
_reflns_number_total             3871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03715_si_002.cif
_cod_data_source_block           PbSe_pyridine
_cod_database_code               4517354
_shelx_res_checksum              43335
_shelx_hkl_checksum              73256