Shedding Light on the Stability and Structure‒Property Relationships of Two-Dimensional Hybrid Lead Bromide Perovskites
Vasileiadou, Eugenia S.; Hadar, Ido; Kepenekian, Mikaël; Even, Jacky; Tu, Qing; Malliakas, Christos D.; Friedrich, Daniel; Spanopoulos, Ioannis; Hoffman, Justin M.; Dravid, Vinayak P.; Kanatzidis, Mercouri G.; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.1c01129

data_4003960
_publ_section_title
;
 Shedding Light on the Stability and Structure--Property Relationships of
 Two-Dimensional Hybrid Lead Bromide Perovskites
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.1c01129
_journal_year                    2021
_chemical_formula_analytical     'Hexylammonium Methylammonium Lead Bromide'
_chemical_formula_iupac          (CH3(CH2)5NH3)2(CH3NH3)Pb2Br7
_chemical_formula_moiety         'C6 H16 Br7 N Pb2, C H6 N, C6 H16 N'
_chemical_formula_sum            'C13 H38 Br7 N3 Pb2'
_chemical_formula_weight         1210.2
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_cell_angle_alpha                90
_cell_angle_beta                 90.852(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   46.069(5)
_cell_length_b                   8.2722(5)
_cell_length_c                   8.3454(12)
_cell_measurement_reflns_used    2261
_cell_measurement_temperature    273.01(15)
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      3.48
_cell_volume                     3180.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_diffrn_ambient_temperature      273.01
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.96
_diffrn_measured_fraction_theta_max 0.76
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10873
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         30.98
_diffrn_reflns_theta_min         2.5
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    19.375
_exptl_absorpt_correction_T_max  0.013
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow plate'
_exptl_crystal_density_diffrn    2.5277
_exptl_crystal_description       'light yellow plate'
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.038
_refine_diff_density_max         2.92
_refine_diff_density_min         -1.08
_refine_ls_abs_structure_details
;
  2128 of Friedel pairs used in the refinement
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    3.50
_refine_ls_goodness_of_fit_ref   2.11
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    167
_refine_ls_number_parameters     133
_refine_ls_number_reflns         5951
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1832
_refine_ls_R_factor_gt           0.0897
_refine_ls_shift/su_max          0.1527
_refine_ls_shift/su_mean         0.2167
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0004I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.2068
_reflns_number_gt                1873
_reflns_number_total             5951
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            cm1c01129_si_001.cif
_cod_data_source_block           C6BrN2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C13 H38 N3 Pb2 Br7'
_cod_database_code               4003960
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1n1(0.2413) H2n1(0.2413) H3n1(0.2413) H1c1(0.2413) H2c1(0.2413)
 H3c1(0.2413) H1n2(0.3861) H2n2(0.3861) H3n2(0.3861) H1c3(0.3861) H2c3(0.3861)
 H1c2(0.3861) H2c2(0.3861) H1c4(0.3861) H2c4(0.3861) H1c6(0.3861) H2c6(0.3861)
 H1c5(0.3861) H2c5(0.3861) H1c7(0.3861) H2c7(0.3861) H3c7(0.3861) H1n3(0.3753)
 H2n3(0.3753) H3n3(0.3753) H1c8(0.3753) H2c8(0.3753) H1c9(0.3753) H2c9(0.3753)
 H1(0.3753) H2(0.3753) H3(0.3753) H4(0.3753) H5(0.3753) H6(0.3753) H7(0.3753)
 H8(0.3753) H9(0.3753)
 Fixed X: H1n1(0.079655) H2n1(0.051367) H3n1(0.054913) H1c1(0.052927)
 H2c1(0.054816) H3c1(0.083279) H1n2(-0.047144) H2n2(-0.025529) H3n2(-0.037161)
 H1c3(-0.106794) H2c3(-0.090834) H1c2(-0.059932) H2c2(-0.064985) H1c4(-
 0.087855) H2c4(-0.11016) H1c6(-0.102875) H2c6(-0.126985) H1c5(-0.14589) H2c5(-
 0.12896) H1c7(-0.156128) H2c7(-0.130722) H3c7(-0.152168) H1n3(0.194949)
 H2n3(0.201124) H3n3(0.201052) H1c8(0.245048) H2c8(0.239579) H1c9(0.244312)
 H2c9(0.272884) H1(0.235904) H2(0.24401) H3(0.287297) H4(0.291498) H5(0.265095)
 H6(0.262908) H7(0.305564) H8(0.305042) H9(0.318753)
 Fixed Y: H1n1(-0.342492) H2n1(-0.388003) H3n1(-0.264608) H1c1(-0.088363)
 H2c1(-0.226047) H3c1(-0.154752) H1n2(0.13612) H2n2(0.204575) H3n2(0.296099)
 H1c3(0.304239) H2c3(0.159775) H1c2(0.259186) H2c2(0.404566) H1c4(0.08363)
 H2c4(0.007663) H1c6(0.386427) H2c6(0.400799) H1c5(0.164657) H2c5(0.140699)
 H1c7(0.373657) H2c7(0.491728) H3c7(0.535413) H1n3(0.290914) H2n3(0.169936)
 H3n3(0.130203) H1c8(0.203119) H2c8(0.360935) H1c9(0.069177) H2c9(0.158362)
 H1(0.238738) H2(0.387305) H3(0.398096) H4(0.210834) H5(0.369329) H6(0.181498)
 H7(0.146567) H8(0.329152) H9(0.278027)
 Fixed Z: H1n1(0.15802) H2n1(0.206362) H3n1(0.089874) H1c1(0.273452)
 H2c1(0.402264) H3c1(0.329694) H1n2(-0.161764) H2n2(-0.260697) H3n2(-0.132699)
 H1c3(-0.257728) H2c3(-0.172654) H1c2(-0.424955) H2c2(-0.307833) H1c4(-
 0.472451) H2c4(-0.354052) H1c6(-0.475006) H2c6(-0.608792) H1c5(-0.439279)
 H2c5(-0.599118) H1c7(-0.345208) H2c7(-0.299243) H3c7(-0.440285) H1n3(0.723342)
 H2n3(0.607921) H3n3(0.773534) H1c8(0.815127) H2c8(0.714996) H1c9(0.552437)
 H2c9(0.605695) H1(0.361167) H2(0.469452) H3(0.377081) H4(0.394251)
 H5(0.134226) H6(0.155548) H7(0.06153) H8(0.011249) H9(0.176664)
;