Materials discovery and design limits in MDABCO perovskites
Gale, Samuel David; Lloyd, Harry James; Male, Louise; Warren, Mark R.; Saunders, Lucy K.; Anderson, P. A.; Yeung, Hamish Hei-Man; CrystEngComm  (2022) –; doi:10.1039/D2CE00848C

data_7245344
_publ_section_title
;
 Materials discovery and design limits in MDABCO perovskites
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00848C
_journal_year                    2022
_chemical_formula_moiety         'Cs1 I3, C7 H16 N2'
_chemical_formula_sum            'C7 H16 Cs I3 N2'
_chemical_formula_weight         641.83
_chemical_name_systematic        '[MDABCO]CsI3'
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-06-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2022-06-22 deposited with the CCDC.	2022-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   9.8648(5)
_cell_length_b                   9.8648(5)
_cell_length_c                   13.7921(17)
_cell_measurement_reflns_used    488
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      18.521918518097653
_cell_measurement_theta_min      2.83576388824828
_cell_volume                     1162.35(17)
_computing_data_reduction
;
DIALS 3.9.0-1-ge664cc1ff-release (Winter, G. et al., 2018)
dials.scale (Beilsten-Edmands, J. et al., 2020)
XIA2 3.9.0 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.825
_diffrn_measured_fraction_theta_max 0.825
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.534
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.825
_diffrn_reflns_Laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            604
_diffrn_reflns_point_group_measured_fraction_full 0.552
_diffrn_reflns_point_group_measured_fraction_max 0.552
_diffrn_reflns_theta_full        18.528
_diffrn_reflns_theta_max         18.528
_diffrn_reflns_theta_min         2.852
_exptl_absorpt_coefficient_mu    3.911
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9961847627764093
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIALS 3.9.0-1-ge664cc1ff-release
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.751
_exptl_crystal_description       plate
_exptl_crystal_F_000             858
_exptl_crystal_preparation
'Dissolve CsI, MDABCO-I (stoichiometric ammounts) in water then add HI (6x stoichiometric ammount). Powder should form instantly.'
_exptl_crystal_recrystallization_method
'Evaporation of water-based solution on a microscope slide, leaves plate-like crystals to form.'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.015
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.224
_refine_ls_abs_structure_details
;
 Flack x determined using 129 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         510
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0648P)^2^+23.7121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.339
_reflns_Friedel_fraction_full    0.279
_reflns_Friedel_fraction_max     0.279
_reflns_number_gt                509
_reflns_number_total             510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00848c2.cif
_cod_data_source_block           MDABCOCsI3
_cod_original_cell_volume        1162.35(18)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7245344
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.696
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.819(5)
 0.181(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H) groups
3. Rigid body (RIGU) restrains
 C3, N1, H1, C1, C2, H1A, H1B, N2, H2A, H2B, H3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4.a Riding coordinates:
 N1(H1), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B)
;
_shelx_res_checksum              9107
_shelx_hkl_checksum              79922
_olex2_submission_original_sample_id '[MDABCO]CsI3'
_olex2_submission_special_instructions 'No special instructions were received'