Tracking the dimensional conversion process of semiconducting lead bromide perovskites by mass spectroscopy, powder X-ray diffraction, microcalorimetry and crystallography.
Hu, Yue-Qiao; Hui, Hong-Yan; Wen, Hong-Qiang; Wang, Yanyan; Lin, Wei-Quan; Yang, De-Suo; Feng, Guo-Dong; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12888–12894; doi:10.1039/c9dt02068c

data_7700640
_publ_section_title
;
 Tracking the dimensional conversion process of semiconducting lead
 bromide perovskites by mass spectroscopy, powder X-ray diffraction,
 microcalorimetry and crystallography.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12888
_journal_page_last               12894
_journal_paper_doi               10.1039/c9dt02068c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '0.15(Br16 Pb4), 0.62(C4 H14 N2 S2)'
_chemical_formula_sum            'C2.46 H8.62 Br2.46 N1.23 Pb0.62 S1.23'
_chemical_formula_weight         419.15
_chemical_name_common            2
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-15 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.983(2)
_cell_angle_gamma                90
_cell_formula_units_Z            13
_cell_length_a                   11.3898(3)
_cell_length_b                   11.6104(3)
_cell_length_c                   22.8884(6)
_cell_measurement_reflns_used    7311
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.8670
_cell_measurement_theta_min      2.4900
_cell_volume                     3026.32(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.789
_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    -13.00  77.00   0.50    3.00    --    4.91  63.00  -0.00  180
  2  \w    -18.00  33.00   0.50    3.00    --    4.91 -99.00-180.00  102
  3  \w    -11.00  19.00   0.50    3.00    --   -7.10 -99.00-150.00   60
  4  \w    -60.00  21.00   0.50    3.00    --    4.91 -63.00-137.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0128839000
_diffrn_orient_matrix_UB_12      -0.0158598000
_diffrn_orient_matrix_UB_13      -0.0291339000
_diffrn_orient_matrix_UB_21      -0.0399693000
_diffrn_orient_matrix_UB_22      0.0422992000
_diffrn_orient_matrix_UB_23      -0.0105842000
_diffrn_orient_matrix_UB_31      0.0459865000
_diffrn_orient_matrix_UB_32      0.0411240000
_diffrn_orient_matrix_UB_33      -0.0003449000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.789
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12759
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.890
_diffrn_reflns_theta_min         2.505
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    21.956
_exptl_absorpt_correction_T_max  0.451
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.990
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.042
_exptl_transmission_factor_max   0.451
_exptl_transmission_factor_min   0.242
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         3766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+3.7890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3369
_reflns_number_total             3766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02068c2.cif
_cod_data_source_block           pbbr-2d-20190713
_cod_depositor_comments
'Adding full bibliography for 7700639--7700640.cif.'
_cod_database_code               7700640
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C4H14Br4N2PbS2
_shelx_estimated_absorpt_t_max   0.398
_shelx_estimated_absorpt_t_min   0.218
_exptl_absorpt_special_details   R(int)
_reflns_odcompleteness_completeness 99.88
_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,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(HF,HG), C1(HH,HI), C3(HJ,HK), C2(HL,HM)
2.b Idealised Me refined as rotating group:
 N1(H,HA,HB), N2(HC,HD,HE)
;
_shelx_res_checksum              14393
_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 1.927
_oxdiff_exptl_absorpt_empirical_full_min 0.560