Metal-free enantiomorphic perovskite [dabcoH<sub>2</sub>]<sup>2+</sup>[H<sub>3</sub>O]<sup>+</sup>Br<sup>-</sup> <sub>3</sub> and its one-dimensional polar polymorph.
Budzianowski, Armand; Petřiček, Vaclav; Katrusiak, Andrzej; IUCrJ 9 (2022) 544–550; doi:10.1107/S2052252522006406

data_1571164
_publ_section_title
;
 Metal-free enantiomorphic perovskite
 [dabcoH<sub>2</sub>]<sup>2+</sup>[H<sub>3</sub>O]<sup>+</sup>Br<sup>-</sup>
 <sub>3</sub> and its one-dimensional polar polymorph.
;
_journal_coeditor_code           CT5016
_journal_issue                   'Pt 5'
_journal_name_full               IUCrJ
_journal_page_first              544
_journal_page_last               550
_journal_paper_doi               10.1107/S2052252522006406
_journal_volume                  9
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 H14 N2, 3(Br), H3 O'
_chemical_formula_sum            'C6 H17 Br3 N2 O'
_chemical_formula_weight         372.94
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-04-20 deposited with the CCDC. 2022-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.5838(3)
_cell_length_b                   9.5838(3)
_cell_length_c                   23.2270(8)
_cell_measurement_reflns_used    3200
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.3070
_cell_measurement_theta_min      3.0150
_cell_volume                     1847.56(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection
;
CrysAlis Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
;
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics
;
X-Seed (Barbour, 2001) 
ShelXle (Hubschle et al., 2011)
VESTA ( Momma & Izumi, 2011)
;
_computing_structure_refinement
;
SHELXL-2016/6 (Sheldrick, 2016)
JANA2006
;
_computing_structure_solution
;
SHELXS-2013/1 (Sheldrick, 1990)
JANA2006
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1929
_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.253
_diffrn_reflns_theta_min         2.454
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.792
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 737 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3159
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0200P)^2^+0.7694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.687
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                2323
_reflns_number_total             3159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ct5016.cif
_cod_data_source_block           dhbr1af_41001
_cod_original_cell_volume        1847.56(13)
_cod_database_code               1571164
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.441
_shelx_estimated_absorpt_t_max   0.441
_shelx_res_checksum              83519
_shelx_hkl_checksum              54638