Post-synthetic halide conversion and selective halogen capture in hybrid perovskites
Solis-Ibarra, D.; Smith, I. C.; Karunadasa, H. I.; Chem. Sci. 6 (2015) 4054–; doi:10.1039/C5SC01135C

data_1519436
_publ_section_title
;
 Post-synthetic halide conversion and selective halogen capture in hybrid
 perovskites
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4054
_journal_paper_doi               10.1039/C5SC01135C
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'Br4 Pb, 2(C4 H10 Cl2 N)'
_chemical_formula_sum            'C8 H20 Br4 Cl4 N2 Pb'
_chemical_formula_weight         812.89
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-02-11 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                97.337(5)
_cell_angle_beta                 96.252(5)
_cell_angle_gamma                90.184(4)
_cell_formula_units_Z            2
_cell_length_a                   7.792(3)
_cell_length_b                   8.315(3)
_cell_length_c                   16.462(6)
_cell_measurement_reflns_used    3306
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      3.47
_cell_volume                     1051.4(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ALS Beamline 11.3.1'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.68880
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9611
_diffrn_reflns_theta_full        24.83
_diffrn_reflns_theta_max         24.83
_diffrn_reflns_theta_min         2.70
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.833
_exptl_absorpt_correction_T_max  0.2643
_exptl_absorpt_correction_T_min  0.1591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1707 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.6020.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water, methanol'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.940
_refine_diff_density_min         -1.839
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+3.8320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                3206
_reflns_number_total             3982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc01135c3.cif
_cod_data_source_block           final1
_cod_depositor_comments
'Adding full bibliography for 1519436--1519438.cif.'
_cod_database_code               1519436
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'