#------------------------------------------------------------------------------
#$Date: 2019-10-29 23:15:44 +0200 (Tue, 29 Oct 2019) $
#$Revision: 220401 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/29/4002977.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_4002977
loop_
_publ_author_name
'Pious, Johnpaul K.'
'Katre, Ankita'
'Muthu, Chinnadurai'
'Chakraborty, Sudip'
'Krishna, Swathi'
'Nair, Vijayakumar C.'
_publ_section_title
;
 Zero-Dimensional Lead-Free Hybrid Perovskite-like Material with a
 Quantum-Well Structure
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1941
_journal_paper_doi               10.1021/acs.chemmater.8b04642
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         'Bi2 I10, 2(C3 H12 N2), 2(O)'
_chemical_formula_sum            'C6 H24 Bi2 I10 N4 O2'
_chemical_formula_weight         1871.25
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.7769(7)
_cell_length_b                   14.7769(7)
_cell_length_c                   13.6748(9)
_cell_measurement_reflns_used    7127
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.08
_cell_measurement_theta_min      2.76
_cell_volume                     2585.9(2)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2013/5 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker KAPPA APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            44044
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.134
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    19.157
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.605
_exptl_crystal_density_meas      3.604
_exptl_crystal_density_method    NONE
_exptl_crystal_description       needle
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.515
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.216
_refine_ls_abs_structure_details
;
 Flack x determined using 1036 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         3042
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0319
_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/[σ²(Fo²)+(0.0239P)²+6.4649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2613
_reflns_number_total             3042
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm8b04642_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2585.9(3)
_cod_database_code               4002977
_shelx_shelxl_version_number     2017/1
_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   0.955
_shelx_estimated_absorpt_t_max   0.995
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
'y, x, -z'
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
C2 C 1.699(3) 0.940(2) 1.0365(19) 0.152(16) Uani 1 1 d . . .
H2A H 1.754290 0.924649 1.020233 0.182 Uiso 1 1 calc R U .
H2B H 1.697606 0.985232 0.986421 0.182 Uiso 1 1 calc R U .
C3 C 1.598(3) 0.842(3) 1.0390(18) 0.187(18) Uani 1 1 d D . .
H3A H 1.609442 0.791004 1.073938 0.225 Uiso 1 1 calc R U .
H3B H 1.551546 0.854621 1.078685 0.225 Uiso 1 1 calc R U .
C4 C 1.544(3) 0.793(2) 0.9517(17) 0.151(14) Uani 1 1 d D . .
H4A H 1.527560 0.841004 0.918630 0.181 Uiso 1 1 calc R U .
H4B H 1.591516 0.783405 0.909714 0.181 Uiso 1 1 calc R U .
N1 N 1.7213(13) 0.9920(11) 1.1312(12) 0.076(5) Uani 1 1 d . . .
H1A H 1.782492 1.051064 1.128683 0.114 Uiso 1 1 calc R U .
H1B H 1.671126 1.006467 1.145728 0.114 Uiso 1 1 calc R U .
H1C H 1.723580 0.950405 1.177017 0.114 Uiso 1 1 calc R U .
N2 N 1.4533(16) 0.698(2) 0.9595(15) 0.137(10) Uani 1 1 d . . .
H2C H 1.426660 0.675801 0.900218 0.206 Uiso 1 1 calc R U .
H2D H 1.466967 0.652098 0.987550 0.206 Uiso 1 1 calc R U .
H2E H 1.407423 0.705723 0.995852 0.206 Uiso 1 1 calc R U .
I1 I 1.000000 0.17635(10) 1.166667 0.0505(4) Uani 1 2 d S T P
I2 I 1.24173(9) 0.42164(9) 0.99877(8) 0.0561(3) Uani 1 1 d . . .
I3 I 0.97959(12) 0.15509(11) 0.86204(11) 0.0795(4) Uani 1 1 d . . .
I4 I 1.01231(9) 0.46637(10) 0.83239(8) 0.0603(3) Uani 1 1 d . . .
I5 I 0.76393(8) 0.22182(10) 0.99832(8) 0.0593(3) Uani 1 1 d . . .
I6 I 1.000000 0.47294(11) 1.166667 0.0576(5) Uani 1 2 d S T P
Bi1 Bi 0.99984(5) 0.32125(5) 0.99353(4) 0.04101(17) Uani 1 1 d . . .
O1' O 1.3569(13) 0.6564(11) 1.1455(11) 0.096(5) Uani 1 1 d . . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 '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
_geom_angle_site_symmetry_3
N1 C2 C3 110(2) .
C4 C3 C2 121(3) .
N2 C4 C3 118(3) .
Bi1 I1 Bi1 95.72(4) 5_767
Bi1 I6 Bi1 93.17(5) 5_767
I3 Bi1 I4 95.26(4) .
I3 Bi1 I5 89.78(4) .
I4 Bi1 I5 90.40(3) .
I3 Bi1 I2 91.45(4) .
I4 Bi1 I2 91.75(3) .
I5 Bi1 I2 177.41(3) .
I3 Bi1 I1 85.83(4) .
I4 Bi1 I1 176.82(3) .
I5 Bi1 I1 92.59(3) .
I2 Bi1 I1 85.23(3) .
I3 Bi1 I6 170.02(4) .
I4 Bi1 I6 93.61(4) .
I5 Bi1 I6 85.57(3) .
I2 Bi1 I6 92.85(2) .
I1 Bi1 I6 85.56(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C2 N1 1.46(2) .
C2 C3 1.47(4) .
C3 C4 1.418(18) .
C4 N2 1.38(3) .
I1 Bi1 3.1930(12) .
I1 Bi1 3.1930(12) 5_767
I2 Bi1 3.1112(12) .
I3 Bi1 2.9355(13) .
I4 Bi1 3.0155(12) .
I5 Bi1 3.0322(12) .
I6 Bi1 3.2595(12) .
I6 Bi1 3.2596(12) 5_767
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2B I5 0.97 3.13 3.82(3) 129.6 1_665 yes
C4 H4A I6 0.97 3.07 4.04(3) 174.5 3_774 yes
N1 H1A I1 0.89 2.84 3.661(16) 153.6 1_665 yes
N1 H1B I4 0.89 3.08 3.957(18) 167.0 6_657 yes
N1 H1C I2 0.89 2.95 3.618(15) 133.7 2_755 yes
N1 H1C I3 0.89 3.17 3.842(17) 133.5 2_755 yes
N2 H2C O1' 0.89 2.08 2.83(2) 142.7 3_774 yes
N2 H2D I4 0.89 3.30 4.14(3) 156.6 2_755 yes
N2 H2E I5 0.89 3.26 4.04(2) 147.0 6_657 yes
N2 H2E O1' 0.89 2.18 2.83(3) 129.7 . yes
C2 H2B I5 0.97 3.13 3.82(3) 129.6 1_665 yes
C4 H4A I6 0.97 3.07 4.04(3) 174.5 3_774 yes
N1 H1A I1 0.89 2.84 3.661(16) 153.6 1_665 yes
N1 H1B I4 0.89 3.08 3.957(18) 167.0 6_657 yes
N1 H1C I2 0.89 2.95 3.618(15) 133.7 2_755 yes
N1 H1C I3 0.89 3.17 3.842(17) 133.5 2_755 yes
N2 H2C O1' 0.89 2.08 2.83(2) 142.7 3_774 yes
N2 H2D I4 0.89 3.30 4.14(3) 156.6 2_755 yes
N2 H2D I4 0.89 3.30 3.75(2) 114.2 4_666 yes
N2 H2E I5 0.89 3.26 4.04(2) 147.0 6_657 yes
N2 H2E O1' 0.89 2.18 2.83(3) 129.7 . yes
