#------------------------------------------------------------------------------
#$Date: 2019-07-31 07:41:19 +0300 (Wed, 31 Jul 2019) $
#$Revision: 217323 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/30/2243036.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243036
loop_
_publ_author_name
'Ferrandin, Sarah'
'Slawin, Alexandra M. Z.'
'Harrison, William T. A.'
_publ_section_title
;
 Syntheses and crystal structures of a new family of hybrid perovskites:
 C₅H₁₄N₂·ABr₃·0.5H₂O (A = K, Rb, Cs)
;
_journal_coeditor_code           VN2151
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1243
_journal_page_last               1248
_journal_paper_doi               10.1107/S2056989019010338
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '(C5 H14 N2) [Rb Br3], 0.5H2 O'
_chemical_formula_moiety         'C5 H14 N2, Rb Br3, 0.5(H2 O)'
_chemical_formula_sum            'C5 H15 Br3 N2 O0.5 Rb'
_chemical_formula_weight         436.39
_chemical_name_systematic
;
Poly[1-methylpiperizine-1,4-diium [tri-μ-bromido-rubidium] hemihydrate]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           38
_space_group_name_Hall           'A 2 -2'
_space_group_name_H-M_alt        'A m m 2'
_symmetry_space_group_name_Hall  'A 2 -2'
_symmetry_space_group_name_H-M   'A m m 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.477(3)
_cell_length_b                   9.5617(19)
_cell_length_c                   9.850(2)
_cell_measurement_reflns_used    2309
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     1269.3(5)
_computing_cell_refinement
;
CrysalisPro (Rigaku, 2017)
;
_computing_data_collection
;
CrysalisPro (Rigaku, 2017)
;
_computing_data_reduction
;
CrysalisPro (Rigaku, 2017)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-7 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Pilatus 200K CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.337
_diffrn_reflns_theta_min         2.969
_exptl_absorpt_coefficient_mu    13.306
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysalisPro; Rigaku, 2017)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.284
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.354
_refine_ls_abs_structure_details
;
Parsons et al. (2013)
;
_refine_ls_abs_structure_Flack   -0.001(13)
_refine_ls_extinction_coef       0.00327(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2014/7 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1264
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0132
_refine_ls_R_factor_gt           0.0128
_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)+(0.0076P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0276
_refine_ls_wR_factor_ref         0.0276
_reflns_number_gt                1244
_reflns_number_total             1264
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            vn2151sup1.cif
_cod_data_source_block           II
_cod_database_code               2243036
_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_min   0.240
_shelx_estimated_absorpt_t_max   0.350
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, z'
'x, -y, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Rb Rb1 0.0000 0.5000 0.09734(7) 0.01032(18) Uani d 1
Rb Rb2 0.5000 0.5000 -0.03670(8) 0.00968(16) Uani d 1
Br Br1 0.0000 0.29829(5) 0.39777(6) 0.01090(14) Uani d 1
Br Br2 0.5000 0.25694(6) 0.21977(6) 0.01073(13) Uani d 1
Br Br3 0.25385(4) 0.5000 0.03510(6) 0.01017(13) Uani d 1
C C1 0.2708(3) 0.6293(4) 0.3838(4) 0.0124(8) Uani d 1
H H1A 0.2118 0.6366 0.3243 0.015 Uiso calc 1
H H1B 0.3130 0.7123 0.3674 0.015 Uiso calc 1
C C2 0.2378(3) 0.6284(4) 0.5303(5) 0.0117(8) Uani d 1
H H2A 0.2966 0.6293 0.5905 0.014 Uiso calc 1
H H2B 0.1980 0.7131 0.5495 0.014 Uiso calc 1
C C3 0.1383(4) 0.5000 0.6996(5) 0.0149(12) Uani d 1
H H3A 0.0985 0.4149 0.7150 0.022 Uiso d 1
H H3B 0.1945 0.5000 0.7635 0.022 Uiso d 1
N N1 0.3274(3) 0.5000 0.3486(5) 0.0107(10) Uani d 1
H H1N 0.3862 0.5000 0.3941 0.013 Uiso calc 1
H H2N 0.3410 0.5000 0.2581 0.013 Uiso calc 1
N N2 0.1766(3) 0.5000 0.5584(4) 0.0087(9) Uani d 1
H H3N 0.1187 0.5000 0.4950 0.010 Uiso calc 1
O O1 0.5000 0.5000 0.5097(5) 0.0109(12) Uani d 1
H H1O 0.5000 0.5749 0.5607 0.013 Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br1 Rb1 Br1 6_554 5_554 110.85(3) ?
Br1 Rb1 Br3 6_554 2_565 84.255(10) ?
Br1 Rb1 Br3 5_554 2_565 84.255(10) ?
Br1 Rb1 Br3 6_554 . 84.255(10) ?
Br1 Rb1 Br3 5_554 . 84.255(10) ?
Br3 Rb1 Br3 2_565 . 159.68(3) ?
Br1 Rb1 Br1 6_554 2_565 157.67(2) ?
Br1 Rb1 Br1 5_554 2_565 91.481(16) ?
Br3 Rb1 Br1 2_565 2_565 98.498(12) ?
Br3 Rb1 Br1 . 2_565 98.498(12) ?
Br1 Rb1 Br1 6_554 . 91.481(15) ?
Br1 Rb1 Br1 5_554 . 157.67(2) ?
Br3 Rb1 Br1 2_565 . 98.498(12) ?
Br3 Rb1 Br1 . . 98.498(12) ?
Br1 Rb1 Br1 2_565 . 66.19(3) ?
Br3 Rb2 Br3 . 2_665 155.93(3) ?
Br3 Rb2 Br2 . 2_665 81.173(14) ?
Br3 Rb2 Br2 2_665 2_665 81.173(13) ?
Br3 Rb2 Br2 . . 81.172(13) ?
Br3 Rb2 Br2 2_665 . 81.173(14) ?
Br2 Rb2 Br2 2_665 . 85.22(3) ?
Br3 Rb2 Br2 . 6_654 98.376(11) ?
Br3 Rb2 Br2 2_665 6_654 98.376(11) ?
Br2 Rb2 Br2 2_665 6_654 176.93(2) ?
Br2 Rb2 Br2 . 6_654 91.702(16) ?
Br3 Rb2 Br2 . 5_554 98.376(11) ?
Br3 Rb2 Br2 2_665 5_554 98.376(11) ?
Br2 Rb2 Br2 2_665 5_554 91.702(16) ?
Br2 Rb2 Br2 . 5_554 176.93(2) ?
Br2 Rb2 Br2 6_654 5_554 91.37(3) ?
Rb1 Br1 Rb1 5_545 . 157.67(2) y
Rb2 Br2 Rb2 . 5_545 176.93(2) y
Rb2 Br3 Rb1 . . 178.12(3) y
N1 C1 C2 . . 111.6(3) ?
N1 C1 H1A . . 109.3 ?
C2 C1 H1A . . 109.3 ?
N1 C1 H1B . . 109.3 ?
C2 C1 H1B . . 109.3 ?
H1A C1 H1B . . 108.0 ?
N2 C2 C1 . . 110.0(3) ?
N2 C2 H2A . . 109.7 ?
C1 C2 H2A . . 109.7 ?
N2 C2 H2B . . 109.7 ?
C1 C2 H2B . . 109.7 ?
H2A C2 H2B . . 108.2 ?
N2 C3 H3A . . 109.5 ?
N2 C3 H3B . . 109.4 ?
H3A C3 H3B . . 108.6 ?
C1 N1 C1 . 4_565 111.7(4) ?
C1 N1 H1N . . 109.3 ?
C1 N1 H1N 4_565 . 109.3 ?
C1 N1 H2N . . 109.3 ?
C1 N1 H2N 4_565 . 109.3 ?
H1N N1 H2N . . 107.9 ?
C3 N2 C2 . . 111.3(3) ?
C3 N2 C2 . 4_565 111.3(3) ?
C2 N2 C2 . 4_565 109.4(4) ?
C3 N2 H3N . . 108.3 ?
C2 N2 H3N . . 108.3 ?
C2 N2 H3N 4_565 . 108.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Rb1 Br1 6_554 3.4639(8) y
Rb1 Br1 5_554 3.4639(8) ?
Rb1 Br1 2_565 3.5323(10) ?
Rb1 Br1 . 3.5323(10) y
Rb1 Br3 2_565 3.4756(9) ?
Rb1 Br3 . 3.4756(9) y
Rb2 Br2 2_665 3.4326(9) ?
Rb2 Br2 . 3.4326(9) y
Rb2 Br2 6_654 3.4336(9) y
Rb2 Br2 5_554 3.4336(9) ?
Rb2 Br3 . 3.3919(9) y
Rb2 Br3 2_665 3.3920(9) ?
Br1 Rb1 5_545 3.4639(8) ?
Br2 Rb2 5_545 3.4336(9) ?
C1 N1 . 1.494(4) ?
C1 C2 . 1.510(6) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 N2 . 1.504(4) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 N2 . 1.484(6) ?
C3 H3A . 0.9868 ?
C3 H3B . 0.9852 ?
N1 C1 4_565 1.494(4) ?
N1 H1N . 0.9100 ?
N1 H2N . 0.9100 ?
N2 C2 4_565 1.504(4) ?
N2 H3N . 1.0000 ?
O1 H1O . 0.8748 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1N O1 . 0.91 1.91 2.816(5) 173
N1 H2N Br3 . 0.91 2.49 3.243(4) 140
N2 H3N Br1 . 1.00 2.68 3.448(4) 134
N2 H3N Br1 2_565 1.00 2.68 3.448(4) 134
O1 H1O Br2 5 0.87 2.34 3.212(3) 173
C1 H1A Br1 2_565 0.99 3.01 3.717(4) 129
C1 H1B Br2 2_665 0.99 2.92 3.652(4) 131
C2 H2B Br1 2_565 0.99 3.06 3.531(4) 111
C2 H2B Br3 5 0.99 2.85 3.560(4) 130
C3 H3A Br1 6 0.99 3.03 3.927(4) 152
C3 H3B Br3 1_556 0.99 2.79 3.653(5) 146
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_site_symmetry_4
_geom_torsion
N1 C1 C2 N2 . -56.8(4)
C2 C1 N1 C1 4_565 53.6(5)
C1 C2 N2 C3 . -176.8(3)
C1 C2 N2 C2 4_565 59.8(5)

_cod_database_fobs_code 2243036
