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_7245345
_publ_section_title
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 Materials discovery and design limits in MDABCO perovskites
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00848C
_journal_year                    2022
_chemical_formula_moiety         'C7 H16 N2, 3(Cl), H4 N'
_chemical_formula_sum            'C7 H20 Cl3 N3'
_chemical_formula_weight         252.61
_chemical_name_systematic        '[MDABCO]NH4Cl3'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-22 deposited with the CCDC.	2022-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.577(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8238(4)
_cell_length_b                   10.1333(3)
_cell_length_c                   16.4441(4)
_cell_measurement_reflns_used    4751
_cell_measurement_temperature    290.3(2)
_cell_measurement_theta_max      72.7830
_cell_measurement_theta_min      3.9770
_cell_volume                     2470.01(12)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      290.3(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3537
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_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   -113.00 -25.00   1.00    4.00    --  -41.39 -57.00  90.00   88
  2  \w    -84.00 -56.00   1.00    4.00    --  -41.39 125.00 -90.00   28
  3  \w   -105.00 -17.00   1.00    4.00    --  -41.39 -38.00 150.00   88
  4  \w     82.00 168.00   1.00   15.97    --  103.11  45.00 120.00   86
  5  \w    105.00 149.00   1.00   15.97    --  103.11  77.00-150.00   44
  6  \w     83.00 144.00   1.00   15.97    --  103.11 178.00  30.00   61
  7  \w     49.00 106.00   1.00   15.97    --  103.11 -45.00 -90.00   57
  8  \w     28.00  56.00   1.00   15.97    --  103.11-111.00-120.00   28
  9  \w     70.00  99.00   1.00   15.97    --  103.11-111.00-120.00   29
 10  \w     83.00 139.00   1.00   15.97    --  103.11  45.00  30.00   56
 11  \w     38.00 119.00   1.00   15.97    --  103.11 -45.00 150.00   81
;
_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      -0.0996789000
_diffrn_orient_matrix_UB_12      -0.0343923000
_diffrn_orient_matrix_UB_13      0.0151426000
_diffrn_orient_matrix_UB_21      0.0211727000
_diffrn_orient_matrix_UB_22      -0.0196684000
_diffrn_orient_matrix_UB_23      0.0911145000
_diffrn_orient_matrix_UB_31      -0.0205236000
_diffrn_orient_matrix_UB_32      0.1467376000
_diffrn_orient_matrix_UB_33      0.0157425000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9853
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.847
_diffrn_reflns_theta_min         3.995
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.439
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.834
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+1.1796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3972
_reflns_number_total             4788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00848c2.cif
_cod_data_source_block           MDABCONH4Cl3
_cod_database_code               7245345
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C7 H20 Cl3 N3'
_shelx_estimated_absorpt_t_max   0.627
_shelx_estimated_absorpt_t_min   0.370
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H,H,H) groups
2. Others
 Sof(N31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(H31D)=1-FVAR(1)
 Sof(N301)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(H30D)=FVAR(1)
3.a Free rotating group:
 N201(H20A,H20B,H20C,H20D), N301(H30A,H30B,H30C,H30D), N31A(H31A,H31B,H31C,H31D)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C105(H10I,
 H10J), C106(H10K,H10L)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C107(H10M,H10N,H10O)
;
_shelx_res_checksum              94660
_shelx_hkl_checksum              99012
_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 1.442
_oxdiff_exptl_absorpt_empirical_full_min 0.798