#------------------------------------------------------------------------------
#$Date: 2022-08-18 00:39:49 +0200 (Thu 18 de Aug de 2022) $
#$Revision: 277292 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/53/7245344.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7245344
loop_
_publ_author_name
'Gale, Samuel David'
'Lloyd, Harry James'
'Male, Louise'
'Warren, Mark R.'
'Saunders, Lucy K.'
'Anderson, P. A.'
'Yeung, Hamish Hei-Man'
_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/[σ²(Fo²)+(0.0648P)²+23.7121P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_olex2_submission_original_sample_id '[MDABCO]CsI3'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I -0.19351(19) -0.3143(2) 0.18402(18) 0.0421(5) Uani 1 1 d . . . . .
Cs1 Cs 0.000000 0.000000 0.0021(4) 0.0552(10) Uani 1 3 d S T P . .
N1 N -0.333333 -0.666667 -0.294(4) 0.048(8) Uani 1 3 d S T P . .
H1 H -0.333333 -0.666667 -0.359930 0.057 Uiso 1 3 d R U P . .
N2 N -0.333333 -0.666667 -0.106(3) 0.037(6) Uani 1 3 d S T P . .
C2 C -0.487(3) -0.685(3) -0.142(3) 0.040(5) Uani 1 1 d . . . . .
H2A H -0.491924 -0.591603 -0.127639 0.048 Uiso 1 1 calc R U . . .
H2B H -0.573877 -0.773247 -0.110606 0.048 Uiso 1 1 calc R U . . .
C1 C -0.499(4) -0.714(4) -0.261(3) 0.054(6) Uani 1 1 d . . . . .
H1A H -0.570721 -0.822969 -0.276183 0.064 Uiso 1 1 calc R U . . .
H1B H -0.535026 -0.650028 -0.292839 0.064 Uiso 1 1 calc R U . . .
C3 C -0.333333 -0.666667 0.012(5) 0.070(13) Uani 1 3 d S T P . .
H3 H -0.236270 -0.658440 0.034673 0.105 Uiso 1 1 d R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -1.1152 1.2808 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -1.2417 1.0917 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0005 0.0017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cs1 I1 Cs1 166.08(8) 4_445 . ?
I1 Cs1 I1 78.89(9) . 2 ?
I1 Cs1 I1 87.86(3) 7_554 3 ?
I1 Cs1 I1 166.08(8) 7_554 . ?
I1 Cs1 I1 102.89(3) 7_554 2 ?
I1 Cs1 I1 78.89(9) 2 3 ?
I1 Cs1 I1 91.00(9) 7_554 9_544 ?
I1 Cs1 I1 87.86(3) 9_544 2 ?
I1 Cs1 I1 102.89(3) 8_444 3 ?
I1 Cs1 I1 78.89(9) . 3 ?
I1 Cs1 I1 91.00(9) 8_444 9_544 ?
I1 Cs1 I1 102.89(3) 9_544 . ?
I1 Cs1 I1 91.00(9) 7_554 8_444 ?
I1 Cs1 I1 87.86(3) 8_444 . ?
I1 Cs1 I1 166.08(8) 8_444 2 ?
I1 Cs1 I1 166.08(8) 9_544 3 ?
C1 N1 H1 107.4 3_545 . ?
C1 N1 H1 107.4 . . ?
C1 N1 H1 107.4 2_445 . ?
C1 N1 C1 111(2) 2_445 3_545 ?
C1 N1 C1 111(2) 3_545 . ?
C1 N1 C1 111(2) 2_445 . ?
C2 N2 C2 109(2) 2_445 . ?
C2 N2 C2 109(2) 3_545 . ?
C2 N2 C2 109(2) 2_445 3_545 ?
C2 N2 C3 110(2) 2_445 . ?
C2 N2 C3 110(2) 3_545 . ?
C2 N2 C3 110(2) . . ?
N2 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
N2 C2 C1 109(3) . . ?
H2A C2 H2B 108.2 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
N1 C1 C2 106(3) . . ?
N1 C1 H1A 110.6 . . ?
N1 C1 H1B 110.6 . . ?
C2 C1 H1A 110.6 . . ?
C2 C1 H1B 110.6 . . ?
H1A C1 H1B 108.7 . . ?
N2 C3 H3 108.6 . . ?
N2 C3 H3 108.623(3) . 2_445 ?
N2 C3 H3 108.623(6) . 3_545 ?
H3 C3 H3 110.3 2_445 3_545 ?
H3 C3 H3 110.3 . 3_545 ?
H3 C3 H3 110.3 . 2_445 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cs1 3.682(3) 4_445 ?
I1 Cs1 3.692(3) . ?
N1 H1 0.9060 . ?
N1 C1 1.53(3) . ?
N1 C1 1.53(3) 2_445 ?
N1 C1 1.53(3) 3_545 ?
N2 C2 1.52(3) 2_445 ?
N2 C2 1.52(3) 3_545 ?
N2 C2 1.52(3) . ?
N2 C3 1.63(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.66(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 H3 0.9705 2_445 ?
C3 H3 0.9705 3_545 ?
C3 H3 0.9704 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C2 C1 N1 -15(3) . . . . ?
C2 N2 C2 C1 -51(3) 2_445 . . . ?
C2 N2 C2 C1 69(3) 3_545 . . . ?
C1 N1 C1 C2 71(3) 2_445 . . . ?
C1 N1 C1 C2 -54(3) 3_545 . . . ?
C3 N2 C2 C1 -170.9(15) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.819(5)
2 0.181(5)
