#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/69/4316943.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_4316943
loop_
_publ_author_name
'Christian Neis'
'David Petry'
'Alexandre Demangeon'
'Bernd Morgenstern'
'Dirk Kuppert'
'Jochen Huppert'
'Stefan Stucky'
'Kaspar Hegetschweiler'
_publ_section_title
;
 Facially Coordinating Triamine Ligands with a Cyclic Backbone: Some
 Structure-Stability Correlations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10092
_journal_page_last               10107
_journal_paper_doi               10.1021/ic101360d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C6 H22 Bi Cl6 N3 O2'
_chemical_formula_weight         589.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.546(2)
_cell_angle_beta                 104.187(2)
_cell_angle_gamma                103.400(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5641(3)
_cell_length_b                   8.4708(4)
_cell_length_c                   14.5577(6)
_cell_measurement_reflns_used    9593
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.73
_cell_measurement_theta_min      2.67
_cell_volume                     865.16(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker X8 Apex, Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54215
_diffrn_reflns_theta_full        47.90
_diffrn_reflns_theta_max         47.90
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    11.114
_exptl_absorpt_correction_T_max  0.2396
_exptl_absorpt_correction_T_min  0.1162
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.988
_refine_diff_density_min         -3.985
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         16068
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0196P)²+0.5456P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0580
_reflns_number_gt                12400
_reflns_number_total             16068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101360d_si_001_2.cif
_cod_data_source_block           H3(MeLa)(BiCl6)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        865.15(6)
_cod_database_code               4316943
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 1.0000 0.0000 0.5000 0.00762(1) Uani 1 2 d S . .
Bi2 Bi 1.0000 0.5000 0.0000 0.00912(1) Uani 1 2 d S . .
Cl1 Cl 1.24379(5) 0.28131(4) 0.48867(3) 0.01345(5) Uani 1 1 d . . .
Cl4 Cl 0.94882(5) 0.67910(4) 0.15355(2) 0.01277(5) Uani 1 1 d . . .
Cl2 Cl 0.79225(5) -0.04510(4) 0.31324(2) 0.01346(5) Uani 1 1 d . . .
Cl3 Cl 1.24189(6) -0.16116(5) 0.45197(3) 0.01698(6) Uani 1 1 d . . .
Cl5 Cl 1.37482(5) 0.58399(6) 0.08071(3) 0.02099(7) Uani 1 1 d . . .
Cl6 Cl 0.98910(6) 0.23924(5) 0.09277(3) 0.01961(7) Uani 1 1 d . . .
C1 C 1.66293(18) 0.38511(15) 0.28645(9) 0.00935(17) Uani 1 1 d . . .
N8 N 1.65615(17) 0.56094(14) 0.28348(9) 0.01107(16) Uani 1 1 d . . .
H8A H 1.6877 0.6180 0.3447 0.017 Uiso 1 1 calc R . .
H8B H 1.5371 0.5622 0.2515 0.017 Uiso 1 1 calc R . .
H8C H 1.7395 0.6088 0.2525 0.017 Uiso 1 1 calc R . .
N6 N 1.47486(17) 0.14098(14) 0.34234(9) 0.01169(17) Uani 1 1 d . . .
H6A H 1.5735 0.0993 0.3348 0.014 Uiso 1 1 calc R . .
H6B H 1.4527 0.1186 0.3995 0.014 Uiso 1 1 calc R . .
C5 C 1.3020(2) 0.05391(19) 0.26161(11) 0.0148(2) Uani 1 1 d . . .
H5A H 1.2039 0.1136 0.2616 0.018 Uiso 1 1 calc R . .
H5B H 1.2518 -0.0585 0.2733 0.018 Uiso 1 1 calc R . .
N3 N 1.40720(19) 0.20366(16) 0.13543(9) 0.01347(19) Uani 1 1 d . . .
H3A H 1.3889 0.1871 0.0698 0.016 Uiso 1 1 calc R . .
H3B H 1.3354 0.2721 0.1496 0.016 Uiso 1 1 calc R . .
C2 C 1.6103(2) 0.28830(18) 0.18360(10) 0.0133(2) Uani 1 1 d . . .
H2A H 1.6556 0.3655 0.1429 0.016 Uiso 1 1 calc R . .
H2B H 1.6817 0.2039 0.1847 0.016 Uiso 1 1 calc R . .
C9 C 1.8691(2) 0.39373(18) 0.33511(12) 0.0151(2) Uani 1 1 d . . .
H9A H 1.9463 0.4256 0.2917 0.023 Uiso 1 1 calc R . .
H9B H 1.8779 0.2854 0.3501 0.023 Uiso 1 1 calc R . .
H9C H 1.9154 0.4757 0.3948 0.023 Uiso 1 1 calc R . .
C7 C 1.5333(2) 0.32406(16) 0.34876(11) 0.0120(2) Uani 1 1 d . . .
H7A H 1.5992 0.3758 0.4168 0.014 Uiso 1 1 calc R . .
H7B H 1.4178 0.3625 0.3296 0.014 Uiso 1 1 calc R . .
C4 C 1.3368(2) 0.04039(18) 0.16380(11) 0.0165(2) Uani 1 1 d . . .
H4A H 1.4307 -0.0236 0.1630 0.020 Uiso 1 1 calc R . .
H4B H 1.2173 -0.0222 0.1150 0.020 Uiso 1 1 calc R . .
O2W O 1.3406(3) 0.0920(2) -0.05438(11) 0.0283(3) Uani 1 1 d D . .
O1W O 1.30243(19) 0.58335(18) 0.29262(9) 0.0214(2) Uani 1 1 d D . .
H2WA H 1.245(3) 0.010(3) -0.068(2) 0.032 Uiso 1 1 d D . .
H1WA H 1.208(3) 0.594(4) 0.2512(18) 0.032 Uiso 1 1 d D . .
H1WB H 1.294(4) 0.633(3) 0.3451(16) 0.032 Uiso 1 1 d D . .
H2WB H 1.347(4) 0.176(3) -0.081(2) 0.032 Uiso 1 1 d 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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
Cl3 Bi1 Cl3 180.000(15) . 2_756 ?
Cl3 Bi1 Cl1 87.141(12) . . ?
Cl3 Bi1 Cl1 92.859(12) 2_756 . ?
Cl3 Bi1 Cl1 92.859(12) . 2_756 ?
Cl3 Bi1 Cl1 87.141(12) 2_756 2_756 ?
Cl1 Bi1 Cl1 180.0 . 2_756 ?
Cl3 Bi1 Cl2 92.281(11) . . ?
Cl3 Bi1 Cl2 87.719(11) 2_756 . ?
Cl1 Bi1 Cl2 93.368(11) . . ?
Cl1 Bi1 Cl2 86.632(11) 2_756 . ?
Cl3 Bi1 Cl2 87.719(11) . 2_756 ?
Cl3 Bi1 Cl2 92.281(11) 2_756 2_756 ?
Cl1 Bi1 Cl2 86.632(11) . 2_756 ?
Cl1 Bi1 Cl2 93.368(11) 2_756 2_756 ?
Cl2 Bi1 Cl2 180.0 . 2_756 ?
Cl5 Bi2 Cl5 180.00(2) 2_765 . ?
Cl5 Bi2 Cl6 85.908(14) 2_765 2_765 ?
Cl5 Bi2 Cl6 94.092(14) . 2_765 ?
Cl5 Bi2 Cl6 94.092(14) 2_765 . ?
Cl5 Bi2 Cl6 85.908(14) . . ?
Cl6 Bi2 Cl6 180.000(16) 2_765 . ?
Cl5 Bi2 Cl4 91.190(12) 2_765 2_765 ?
Cl5 Bi2 Cl4 88.810(12) . 2_765 ?
Cl6 Bi2 Cl4 89.742(12) 2_765 2_765 ?
Cl6 Bi2 Cl4 90.258(12) . 2_765 ?
Cl5 Bi2 Cl4 88.810(12) 2_765 . ?
Cl5 Bi2 Cl4 91.190(12) . . ?
Cl6 Bi2 Cl4 90.258(12) 2_765 . ?
Cl6 Bi2 Cl4 89.742(12) . . ?
Cl4 Bi2 Cl4 180.00(2) 2_765 . ?
N8 C1 C9 105.98(10) . . ?
N8 C1 C2 109.77(11) . . ?
C9 C1 C2 107.86(11) . . ?
N8 C1 C7 104.57(10) . . ?
C9 C1 C7 111.59(12) . . ?
C2 C1 C7 116.55(11) . . ?
C5 N6 C7 114.08(11) . . ?
N6 C5 C4 113.77(12) . . ?
C2 N3 C4 114.46(12) . . ?
N3 C2 C1 118.02(11) . . ?
N6 C7 C1 115.12(10) . . ?
N3 C4 C5 114.25(12) . . ?
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
Bi1 Cl3 2.6958(3) . ?
Bi1 Cl3 2.6958(3) 2_756 ?
Bi1 Cl1 2.7034(3) . ?
Bi1 Cl1 2.7034(3) 2_756 ?
Bi1 Cl2 2.7199(4) . ?
Bi1 Cl2 2.7199(4) 2_756 ?
Bi2 Cl5 2.6771(4) 2_765 ?
Bi2 Cl5 2.6771(4) . ?
Bi2 Cl6 2.7130(4) 2_765 ?
Bi2 Cl6 2.7130(4) . ?
Bi2 Cl4 2.7150(3) 2_765 ?
Bi2 Cl4 2.7150(3) . ?
C1 N8 1.5073(16) . ?
C1 C9 1.5273(19) . ?
C1 C2 1.5328(19) . ?
C1 C7 1.5363(18) . ?
N6 C5 1.4957(19) . ?
N6 C7 1.4961(18) . ?
C5 C4 1.507(2) . ?
N3 C2 1.488(2) . ?
N3 C4 1.5045(19) . ?
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
O2W H2WB Cl5 0.843(17) 2.56(3) 3.1967(17) 133(3) 2_865
O2W H2WA Cl6 0.839(17) 2.350(18) 3.1813(18) 171(3) 2_755
N3 H3A O2W 0.92 1.81 2.699(2) 163.1 .
N3 H3B Cl6 0.92 2.48 3.1622(14) 130.7 .
O1W H1WA Cl4 0.843(17) 2.433(18) 3.2614(14) 168(3) .
O1W H1WB Cl3 0.853(17) 2.370(19) 3.1797(13) 159(3) 1_565
N8 H8B O1W 0.91 2.05 2.7598(17) 134.4 .
N8 H8B Cl5 0.91 2.54 3.2441(13) 134.9 .
N8 H8A Cl1 0.91 2.36 3.2636(13) 169.6 2_866
N8 H8C Cl4 0.91 2.41 3.3072(12) 168.4 1_655
N6 H6A Cl2 0.92 2.33 3.2447(12) 171.4 1_655
N6 H6B Cl3 0.92 2.67 3.1866(13) 116.3 2_856
N6 H6B Cl3 0.92 2.83 3.5245(12) 133.4 .
N6 H6B Cl1 0.92 2.77 3.3490(12) 121.7 .
