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_7245346
_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         'Rb, 3(Br), C7 H16 N2'
_chemical_formula_sum            'C7 H16 Br3 N2 Rb'
_chemical_formula_weight         453.42
_chemical_name_systematic        '[MDABCO]RbBr3'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_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                90
_cell_formula_units_Z            4
_cell_length_a                   14.1838(10)
_cell_length_b                   9.9322(6)
_cell_length_c                   9.6159(6)
_cell_measurement_reflns_used    6619
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      72.4440
_cell_measurement_theta_min      6.2100
_cell_volume                     1354.65(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3537
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00  33.00   1.00    5.23    --  -41.39  38.00-150.00   99
  2  \w    -86.00  -6.00   1.00    5.23    --  -41.39 125.00-150.00   80
  3  \w     27.00  97.00   1.00    5.23    --   41.39-125.00   0.00   70
  4  \w     27.00  97.00   1.00    5.23    --   41.39-125.00  60.00   70
  5  \w    104.00 178.00   1.00   20.92    --  103.11 111.00   0.00   74
  6  \w     74.00 175.00   1.00   20.92    --  103.11  61.00  90.00  101
  7  \w     44.00  72.00   1.00   20.92    --  103.11 -15.00 -90.00   28
  8  \w     78.00 129.00   1.00   20.92    --  103.11 -15.00 -90.00   51
  9  \w     75.00 108.00   1.00   20.92    --  103.11 178.00-180.00   33
 10  \w    140.00 171.00   1.00   20.92    --  103.11  45.00 150.00   31
 11  \w    116.00 159.00   1.00   20.92    --  103.11  45.00-120.00   43
 12  \w     83.00 137.00   1.00   20.92    --  103.11  45.00 150.00   54
 13  \w     14.00 115.00   1.00    5.23    --   41.77  57.00-120.00  101
 14  \w     14.00 115.00   1.00    5.23    --   41.77  57.00-180.00  101
 15  \w     14.00 115.00   1.00    5.23    --   41.77  57.00  90.00  101
 16  \w    -21.00  74.00   1.00    5.23    --   41.77 -77.00 120.00   95
 17  \w     14.00 115.00   1.00    5.23    --   41.77  56.00 -18.00  101
 18  \w     27.00 109.00   1.00   20.92    --  103.11-111.00  30.00   82
 19  \w    103.00 178.00   1.00   20.92    --  103.11  77.00 -60.00   75
 20  \w     74.00 139.00   1.00   20.92    --  103.11  61.00 -90.00   65
 21  \w     77.00 176.00   1.00   20.92    --  103.11  45.00  30.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0000240000
_diffrn_orient_matrix_UB_12      0.1166726000
_diffrn_orient_matrix_UB_13      -0.1055264000
_diffrn_orient_matrix_UB_21      0.0728126000
_diffrn_orient_matrix_UB_22      0.0757574000
_diffrn_orient_matrix_UB_23      0.0895285000
_diffrn_orient_matrix_UB_31      0.0805925000
_diffrn_orient_matrix_UB_32      -0.0685353000
_diffrn_orient_matrix_UB_33      -0.0807905000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11848
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.364
_diffrn_reflns_theta_min         5.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.114
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)

Numerical absorption correction based on gaussian integration over

a multifaceted crystal model

Empirical absorption correction using spherical harmonics,

implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    2.223
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 1046 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_coef       0.00064(7)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2594
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0390P)^2^+1.4495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.919
_reflns_number_gt                2457
_reflns_number_total             2594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00848c2.cif
_cod_data_source_block           MDABCORbBr3
_cod_database_code               7245346
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C7 H16 Rb1 N2 Br3'
_cell_oxdiff_angle_alpha         90.017(4)
_cell_oxdiff_angle_beta          90.017(4)
_cell_oxdiff_angle_gamma         89.985(4)
_cell_oxdiff_length_a            14.1839(8)
_cell_oxdiff_length_b            9.9342(5)
_cell_oxdiff_length_c            9.6138(5)
_cell_oxdiff_measurement_reflns_used 6619
_cell_oxdiff_volume              1354.65(13)
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.313
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              98334
_shelx_hkl_checksum              38757
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.042
_oxdiff_exptl_absorpt_empirical_full_min 0.599