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_7700639
_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         'Br5 Pb, C4 H14 N2 S2, H2 O'
_chemical_formula_sum            'C4 H16 Br5 N2 O Pb S2'
_chemical_formula_weight         779.05
_chemical_name_common            1
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                 104.184(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0824(3)
_cell_length_b                   8.3838(2)
_cell_length_c                   10.9546(4)
_cell_measurement_reflns_used    6529
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      30.9110
_cell_measurement_theta_min      2.4550
_cell_volume                     897.75(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.806
_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    -19.00  15.00   0.50    2.00    --    4.91 -86.00  70.00   68
  2  \w    -18.00  28.00   0.50    2.00    --   -6.94 -99.00  30.00   92
  3  \w    -20.00  28.00   0.50    2.00    --   -6.94 -99.00   0.00   96
  4  \w    -21.00  24.00   0.50    2.00    --    4.91 -99.00-150.00   90
  5  \w    -66.00  21.00   0.50    2.00    --    4.91 -57.00 -30.00  174
  6  \w    -11.00  40.00   0.50    2.00    --    4.91  86.00-171.00  102
;
_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      0.0546462000
_diffrn_orient_matrix_UB_12      0.0480283000
_diffrn_orient_matrix_UB_13      0.0338244000
_diffrn_orient_matrix_UB_21      0.0475630000
_diffrn_orient_matrix_UB_22      -0.0583532000
_diffrn_orient_matrix_UB_23      -0.0091855000
_diffrn_orient_matrix_UB_31      0.0039375000
_diffrn_orient_matrix_UB_32      0.0380177000
_diffrn_orient_matrix_UB_33      -0.0568624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9646
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.700
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.870
_diffrn_reflns_theta_min         2.462
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.739
_exptl_absorpt_correction_T_max  0.649
_exptl_absorpt_correction_T_min  0.348
_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    2.882
_exptl_crystal_description       block
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.023
_exptl_transmission_factor_max   0.649
_exptl_transmission_factor_min   0.348
_refine_diff_density_max         0.875
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details
;
 Flack x determined using 1363 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3953
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0163P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0471
_reflns_Friedel_coverage         0.637
_reflns_Friedel_fraction_full    0.855
_reflns_Friedel_fraction_max     0.581
_reflns_number_gt                3686
_reflns_number_total             3953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02068c2.cif
_cod_data_source_block           190713_1_mo
_cod_depositor_comments
'Adding full bibliography for 7700639--7700640.cif.'
_cod_database_code               7700639
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C4H17Br5N2OPbS2
_shelx_estimated_absorpt_t_max   0.647
_shelx_estimated_absorpt_t_min   0.317
_exptl_absorpt_special_details   R(int)
_reflns_odcompleteness_completeness 99.75
_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
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1F,H1G)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2D,H2E), C3(H3A,H3B), C4(H4A,H4B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              10872
_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 2.834
_oxdiff_exptl_absorpt_empirical_full_min 0.512