Robot-Accelerated Perovskite Investigation and Discovery
Li, Zhi; Najeeb, Mansoor Ani; Alves, Liana; Sherman, Alyssa Z.; Shekar, Venkateswaran; Cruz Parrilla, Peter; Pendleton, Ian M.; Wang, Wesley; Nega, Philip W.; Zeller, Matthias; Schrier, Joshua; Norquist, Alexander J.; Chan, Emory M.; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c01153

data_4003586
_publ_section_title
;
 Robot-Accelerated Perovskite Investigation and Discovery
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c01153
_journal_year                    2020
_chemical_formula_moiety         '2(I3 Pb), I3 Pb, 3(C2 H7 N2)'
_chemical_formula_sum            'C6 H21 I9 N6 Pb3'
_chemical_formula_weight         1940.96
_space_group_crystal_system      trigonal
_space_group_IT_number           157
_space_group_name_Hall           'P 3 -2'
_space_group_name_H-M_alt        'P 3 1 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.2648(6)
_cell_length_b                   15.2648(6)
_cell_length_c                   8.1332(3)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.0767
_cell_measurement_theta_min      2.6685
_cell_volume                     1641.25(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'Apex3 v2018.1-0 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev946 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            39926
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.216
_diffrn_reflns_theta_min         2.504
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    23.820
_exptl_absorpt_correction_T_max  0.1044
_exptl_absorpt_correction_T_min  0.0387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.928
_exptl_crystal_description       rod
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.738
_refine_diff_density_min         -2.709
_refine_diff_density_rms         0.294
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.00058(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         4447
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0012P)^2^+23.5317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3845
_reflns_number_total             4447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01153_si_002.cif
_cod_data_source_block           MAN_101_1_0m
_cod_original_cell_volume        1641.25(14)
_cod_database_code               4003586
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.115
_shelx_estimated_absorpt_t_max   0.252
_shelx_res_checksum              10013
_shelx_hkl_checksum              16036