Melting Temperature Suppression of Layered Hybrid Lead Halide Perovskites via Organic Ammonium Cation Branching
Li, Tianyang; Dunlap-Shohl, Wiley; Reinheimer, Eric W.; LeMagueres, Pierre; Mitzi, David B.; Chemical Science  (2019) –; doi:10.1039/C8SC03863E

data_1550207
_publ_section_title
;
 Melting Temperature Suppression of Layered Hybrid Lead Halide Perovskites
 via Organic Ammonium Cation Branching
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03863E
_journal_year                    2019
_chemical_formula_moiety         '0.5(I8 Pb2), C8 H26 N2'
_chemical_formula_sum            'C8 H26 I4 N2 Pb'
_chemical_formula_weight         865.10
_space_group_crystal_system      tetragonal
_space_group_IT_number           138
_space_group_name_Hall           '-P 4ac 2ac'
_space_group_name_H-M_alt        'P 42/n c m'
_symmetry_space_group_name_Hall  '-P 4ac 2ac'
_symmetry_space_group_name_H-M   'P 42/n c m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-24 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9353(2)
_cell_length_b                   8.9353(2)
_cell_length_c                   24.9636(13)
_cell_measurement_reflns_used    6263
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.2310
_cell_measurement_theta_min      2.7640
_cell_volume                     1993.08(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.3a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.3a (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_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11096
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.804
_diffrn_source                   'microfocused sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.644
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'metallic orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.883
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.749
_refine_diff_density_min         -2.003
_refine_diff_density_rms         0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         972
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          1.026
_refine_ls_shift/su_mean         0.087
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1568P)^2^+7.2173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2229
_refine_ls_wR_factor_ref         0.2263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                905
_reflns_number_total             972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03863e2.cif
_cod_data_source_block           1me-pa_roomt_feb
_cod_original_cell_volume        1993.10(15)
_cod_database_code               1550207
_shelx_shelxl_version_number     2014/7
_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 C(H,H,H) groups
2. Restrained distances
 N1-C3
 1.47 with sigma of 0.02
 C4-C8
 1.54 with sigma of 0.02
 C8-C4 \\sim C4-C3
 with sigma of 0.001
 C5-C3 \\sim C4-C3
 with sigma of 0.001
 C8-C4 \\sim C4-C3 \\sim C5-C3
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C4) = Uanis(C3) = Uanis(N1)
Uanis(C8) = Uanis(C4) = Uanis(C5) = Uanis(C3) = Uanis(N1)
Uanis(C3) = Uanis(C8)
4. Rigid body (RIGU) restrains
 N1, C3, C4, C5, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) C4(0.5) H4A(0.5) H4B(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) H8C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
6.a Ternary CH refined with riding coordinates:
 C3(H3B), C3(H3A)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
6.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              47431
_olex2_submission_special_instructions 'No special instructions were received'