#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/12/4321293.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_4321293
loop_
_publ_author_name
'Jan Näslund'
'Ingmar Persson'
'Magnus Sandstrom'
_publ_contact_author
;
    Prof. Ingmar Persson
    Department of Chemistry, SLU
    P.O.Box 7015
    SE-750 07 Uppsala
    Sweden
;
_publ_contact_author_email       Ingmar.Persson@kemi.slu.se
_publ_contact_author_fax         '+46 18 673476'
_publ_contact_author_phone       '+46 18 671547'
_publ_section_title
;
 Solvation of the Bismuth(III) Ion by Water, Dimethyl Sulfoxide,
 N,N'-Dimethylpropyleneurea, and N,N-Dimethylthioformamide. An EXAFS,
 Large-Angle X-ray Scattering, and Crystallographic Structural Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4012
_journal_page_last               4021
_journal_paper_doi               10.1021/ic000022m
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C36 H72 Bi Cl3 N12 O18'
_chemical_formula_weight         1276.37
_chemical_name_systematic
; 
 hexakis dimethylpropylenurea bismuth(III) perchlorate 
;
_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                103.9390(10)
_cell_angle_beta                 103.9280(10)
_cell_angle_gamma                103.9360(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4290(10)
_cell_length_b                   14.4264(10)
_cell_length_c                   14.4206(10)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      0
_cell_volume                     2681.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      566(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.1017
_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       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14226
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    3.510
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.619
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         9866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0941P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1819
_reflns_number_gt                4264
_reflns_number_total             9866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000022m_1.cif
_cod_data_source_block           bidmpu0m
_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.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C36 H72  Bi Cl3 N12 O18'
_cod_database_code               4321293
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 0.24998(4) 0.75003(4) 0.25006(4) 0.0808(2) Uani 1 1 d . . .
O1 O 0.3917(7) 0.8619(8) 0.2398(7) 0.107(3) Uani 1 1 d . . .
O2 O 0.3582(7) 0.7373(8) 0.3902(7) 0.110(3) Uani 1 1 d . . .
O3 O 0.1403(8) 0.6083(7) 0.2602(8) 0.115(3) Uani 1 1 d . . .
O4 O 0.1096(7) 0.7613(8) 0.1401(7) 0.112(3) Uani 1 1 d . . .
O5 O 0.2627(8) 0.6413(7) 0.1096(7) 0.107(3) Uani 1 1 d . . .
O6 O 0.2380(8) 0.8905(7) 0.3590(7) 0.109(3) Uani 1 1 d . . .
C1 C 0.4650(8) 0.8717(8) 0.2059(9) 0.063(3) Uani 1 1 d . . .
C2 C 0.3715(8) 0.7054(9) 0.4645(8) 0.065(3) Uani 1 1 d . . .
C3 C 0.1270(8) 0.5337(8) 0.2928(9) 0.065(3) Uani 1 1 d . . .
C4 C 0.0372(8) 0.7965(9) 0.1293(8) 0.063(3) Uani 1 1 d . . .
C5 C 0.2943(9) 0.6280(8) 0.0350(8) 0.064(3) Uani 1 1 d . . .
C6 C 0.2063(8) 0.9647(8) 0.3726(8) 0.061(3) Uani 1 1 d . . .
N11 N 0.4558(6) 0.8897(6) 0.1175(7) 0.064(2) Uani 1 1 d . . .
N12 N 0.5531(8) 0.8688(7) 0.2585(7) 0.077(3) Uani 1 1 d . . .
N21 N 0.3909(7) 0.6187(7) 0.4563(6) 0.066(2) Uani 1 1 d . . .
N22 N 0.3673(7) 0.7574(7) 0.5536(8) 0.077(3) Uani 1 1 d . . .
N31 N 0.1106(7) 0.5444(6) 0.3823(7) 0.068(2) Uani 1 1 d . . .
N32 N 0.1321(7) 0.4457(7) 0.2421(7) 0.078(3) Uani 1 1 d . . .
N41 N 0.0448(6) 0.8820(7) 0.1095(7) 0.069(2) Uani 1 1 d . . .
N42 N -0.0531(7) 0.7417(7) 0.1317(7) 0.079(3) Uani 1 1 d . . .
N51 N 0.2415(8) 0.6325(7) -0.0534(7) 0.080(3) Uani 1 1 d . . .
N52 N 0.3819(7) 0.6099(7) 0.0451(6) 0.069(3) Uani 1 1 d . . .
N61 N 0.1176(7) 0.9553(6) 0.3907(7) 0.066(2) Uani 1 1 d . . .
N62 N 0.2576(7) 1.0520(7) 0.3680(7) 0.077(3) Uani 1 1 d . . .
Cl1 Cl 0.8392(3) 0.1610(3) 0.2504(3) 0.0885(10) Uani 1 1 d . . .
O11 O 0.8532(11) 0.1042(11) 0.3105(11) 0.184(6) Uani 1 1 d . . .
O12 O 0.8939(13) 0.1451(11) 0.1878(11) 0.196(6) Uani 1 1 d . . .
O13 O 0.7343(9) 0.1305(11) 0.2008(10) 0.181(6) Uani 1 1 d . . .
O14 O 0.8688(11) 0.2631(8) 0.2988(10) 0.174(5) Uani 1 1 d . . .
Cl2 Cl 0.7502(3) 0.6612(3) 0.3390(3) 0.0872(9) Uani 1 1 d . . .
O21 O 0.6894(11) 0.6495(11) 0.3963(11) 0.174(5) Uani 1 1 d . . .
O22 O 0.7986(10) 0.7653(8) 0.3685(11) 0.180(6) Uani 1 1 d . . .
O23 O 0.6998(10) 0.6329(11) 0.2360(9) 0.179(6) Uani 1 1 d . . .
O24 O 0.8134(11) 0.6080(12) 0.3536(11) 0.186(6) Uani 1 1 d . . .
Cl3 Cl 0.3388(3) 0.2500(3) 0.1610(3) 0.0867(9) Uani 1 1 d . . .
O31 O 0.2361(9) 0.2003(10) 0.1290(11) 0.185(6) Uani 1 1 d . . .
O32 O 0.3928(11) 0.1865(10) 0.1470(11) 0.183(6) Uani 1 1 d . . .
O33 O 0.3514(11) 0.3093(11) 0.1024(12) 0.185(6) Uani 1 1 d . . .
O34 O 0.3673(11) 0.2971(10) 0.2639(9) 0.178(6) Uani 1 1 d . . .
C51 C 0.1389(12) 0.6457(11) -0.0685(11) 0.108(5) Uiso 1 1 d . . .
C42 C -0.0694(12) 0.6406(12) 0.1441(12) 0.115(5) Uiso 1 1 d . . .
C32 C 0.1424(11) 0.4295(11) 0.1392(11) 0.105(4) Uiso 1 1 d . . .
C62 C 0.3581(13) 1.0665(12) 0.3549(12) 0.121(5) Uiso 1 1 d . . .
C43 C -0.0424(10) 0.9199(9) 0.0808(10) 0.090(4) Uiso 1 1 d . . .
C12 C 0.5691(11) 0.8565(11) 0.3604(12) 0.109(5) Uiso 1 1 d . . .
C53 C 0.2782(11) 0.6159(10) -0.1450(11) 0.098(4) Uiso 1 1 d . . .
C13 C 0.6463(11) 0.8869(10) 0.2235(10) 0.098(4) Uiso 1 1 d . . .
C31 C 0.0972(10) 0.6415(10) 0.4383(10) 0.089(4) Uiso 1 1 d . . .
C63 C 0.2228(10) 1.1449(10) 0.3854(10) 0.097(4) Uiso 1 1 d . . .
C52 C 0.4378(10) 0.5949(9) 0.1399(10) 0.087(4) Uiso 1 1 d . . .
C23 C 0.3856(10) 0.7227(10) 0.6458(10) 0.098(4) Uiso 1 1 d . . .
C34 C 0.1131(10) 0.3535(10) 0.2769(10) 0.094(4) Uiso 1 1 d . . .
C21 C 0.4043(10) 0.5630(10) 0.3608(10) 0.089(4) Uiso 1 1 d . . .
C44 C -0.1464(10) 0.7789(10) 0.1136(10) 0.095(4) Uiso 1 1 d . . .
C64 C 0.0777(10) 1.0412(10) 0.4172(10) 0.091(4) Uiso 1 1 d . . .
C11 C 0.3588(10) 0.9041(10) 0.0631(10) 0.090(4) Uiso 1 1 d . . .
C41 C 0.1394(10) 0.9367(9) 0.0952(9) 0.087(4) Uiso 1 1 d . . .
C22 C 0.3558(12) 0.8612(12) 0.5672(12) 0.115(5) Uiso 1 1 d . . .
C54 C 0.4185(10) 0.5812(9) -0.0426(10) 0.089(4) Uiso 1 1 d . . .
C24 C 0.4191(10) 0.5797(9) 0.5410(10) 0.090(4) Uiso 1 1 d . . .
C14 C 0.5418(10) 0.9201(10) 0.0802(10) 0.096(4) Uiso 1 1 d . . .
C33 C 0.0812(10) 0.4592(10) 0.4196(10) 0.098(4) Uiso 1 1 d . . .
C61 C 0.0623(10) 0.8605(10) 0.4039(9) 0.088(4) Uiso 1 1 d . . .
C45 C -0.1105(11) 0.8904(11) 0.1409(11) 0.106(4) Uiso 1 1 d . . .
C15 C 0.6098(11) 0.8610(11) 0.1112(11) 0.103(4) Uiso 1 1 d . . .
C65 C 0.1091(11) 1.1084(10) 0.3594(10) 0.096(4) Uiso 1 1 d . . .
C25 C 0.3615(11) 0.6122(10) 0.6112(10) 0.098(4) Uiso 1 1 d . . .
C35 C 0.1407(11) 0.3886(11) 0.3885(11) 0.103(4) Uiso 1 1 d . . .
C55 C 0.3879(11) 0.6407(11) -0.1105(11) 0.106(5) Uiso 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'
O O 0.0106 0.0060 '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'
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
O2 Bi1 O6 86.4(3) . . ?
O2 Bi1 O4 162.4(3) . . ?
O6 Bi1 O4 83.6(4) . . ?
O2 Bi1 O5 107.0(3) . . ?
O6 Bi1 O5 162.2(3) . . ?
O4 Bi1 O5 86.0(3) . . ?
O2 Bi1 O3 83.4(4) . . ?
O6 Bi1 O3 107.8(3) . . ?
O4 Bi1 O3 85.9(4) . . ?
O5 Bi1 O3 85.8(3) . . ?
O2 Bi1 O1 86.3(3) . . ?
O6 Bi1 O1 85.4(3) . . ?
O4 Bi1 O1 107.2(3) . . ?
O5 Bi1 O1 83.9(4) . . ?
O3 Bi1 O1 162.6(3) . . ?
C1 O1 Bi1 146.4(9) . . ?
C2 O2 Bi1 149.5(9) . . ?
C3 O3 Bi1 149.0(9) . . ?
C4 O4 Bi1 147.2(8) . . ?
C5 O5 Bi1 149.5(9) . . ?
C6 O6 Bi1 149.5(9) . . ?
O1 C1 N12 120.9(11) . . ?
O1 C1 N11 119.8(10) . . ?
N12 C1 N11 119.2(9) . . ?
O2 C2 N21 120.0(11) . . ?
O2 C2 N22 121.6(10) . . ?
N21 C2 N22 118.5(9) . . ?
O3 C3 N32 121.4(11) . . ?
O3 C3 N31 119.4(10) . . ?
N32 C3 N31 119.1(10) . . ?
O4 C4 N41 121.5(11) . . ?
O4 C4 N42 119.2(10) . . ?
N41 C4 N42 119.2(9) . . ?
O5 C5 N52 118.8(11) . . ?
O5 C5 N51 121.0(10) . . ?
N52 C5 N51 120.2(10) . . ?
O6 C6 N62 121.2(10) . . ?
O6 C6 N61 119.6(10) . . ?
N62 C6 N61 119.2(9) . . ?
C1 N11 C14 123.7(9) . . ?
C1 N11 C11 119.1(9) . . ?
C14 N11 C11 115.7(9) . . ?
C1 N12 C12 121.2(10) . . ?
C1 N12 C13 122.8(10) . . ?
C12 N12 C13 115.8(10) . . ?
C2 N21 C24 124.6(9) . . ?
C2 N21 C21 119.9(9) . . ?
C24 N21 C21 114.6(9) . . ?
C2 N22 C23 123.1(9) . . ?
C2 N22 C22 119.1(10) . . ?
C23 N22 C22 117.4(11) . . ?
C3 N31 C33 123.0(9) . . ?
C3 N31 C31 120.2(9) . . ?
C33 N31 C31 115.3(9) . . ?
C3 N32 C32 120.1(10) . . ?
C3 N32 C34 123.0(10) . . ?
C32 N32 C34 116.3(10) . . ?
C4 N41 C41 119.6(9) . . ?
C4 N41 C43 123.9(10) . . ?
C41 N41 C43 115.5(9) . . ?
C4 N42 C42 121.9(10) . . ?
C4 N42 C44 121.5(9) . . ?
C42 N42 C44 116.4(11) . . ?
C5 N51 C51 121.0(10) . . ?
C5 N51 C53 121.8(10) . . ?
C51 N51 C53 117.1(10) . . ?
C5 N52 C54 122.0(9) . . ?
C5 N52 C52 121.3(9) . . ?
C54 N52 C52 115.4(9) . . ?
C6 N61 C61 120.2(9) . . ?
C6 N61 C64 123.7(9) . . ?
C61 N61 C64 115.1(9) . . ?
C6 N62 C62 120.4(10) . . ?
C6 N62 C63 123.1(10) . . ?
C62 N62 C63 116.3(11) . . ?
O11 Cl1 O12 106.7(9) . . ?
O11 Cl1 O14 115.5(9) . . ?
O12 Cl1 O14 107.7(9) . . ?
O11 Cl1 O13 106.6(9) . . ?
O12 Cl1 O13 114.0(10) . . ?
O14 Cl1 O13 106.6(9) . . ?
O24 Cl2 O21 109.3(9) . . ?
O24 Cl2 O23 108.7(9) . . ?
O21 Cl2 O23 114.6(9) . . ?
O24 Cl2 O22 113.6(10) . . ?
O21 Cl2 O22 105.3(9) . . ?
O23 Cl2 O22 105.4(9) . . ?
O32 Cl3 O33 108.3(9) . . ?
O32 Cl3 O34 106.7(9) . . ?
O33 Cl3 O34 117.3(9) . . ?
O32 Cl3 O31 112.7(9) . . ?
O33 Cl3 O31 105.1(9) . . ?
O34 Cl3 O31 107.0(9) . . ?
N41 C43 C45 106.7(11) . . ?
C55 C53 N51 108.9(11) . . ?
C15 C13 N12 107.3(11) . . ?
C65 C63 N62 107.5(11) . . ?
C25 C23 N22 108.1(11) . . ?
C35 C34 N32 108.0(11) . . ?
C45 C44 N42 108.4(11) . . ?
C65 C64 N61 106.3(11) . . ?
N52 C54 C55 106.8(10) . . ?
N21 C24 C25 106.1(10) . . ?
N11 C14 C15 105.4(11) . . ?
N31 C33 C35 106.5(11) . . ?
C44 C45 C43 109.0(12) . . ?
C13 C15 C14 110.7(12) . . ?
C64 C65 C63 111.0(12) . . ?
C23 C25 C24 111.4(13) . . ?
C34 C35 C33 109.0(12) . . ?
C53 C55 C54 110.2(13) . . ?
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 O2 2.314(8) . ?
Bi1 O6 2.317(8) . ?
Bi1 O4 2.320(9) . ?
Bi1 O5 2.321(8) . ?
Bi1 O3 2.324(9) . ?
Bi1 O1 2.341(9) . ?
O1 C1 1.260(12) . ?
O2 C2 1.256(12) . ?
O3 C3 1.267(12) . ?
O4 C4 1.261(11) . ?
O5 C5 1.257(12) . ?
O6 C6 1.254(11) . ?
C1 N12 1.330(13) . ?
C1 N11 1.343(13) . ?
C2 N21 1.331(12) . ?
C2 N22 1.345(13) . ?
C3 N32 1.333(13) . ?
C3 N31 1.346(13) . ?
C4 N41 1.316(12) . ?
C4 N42 1.364(13) . ?
C5 N52 1.332(12) . ?
C5 N51 1.344(13) . ?
C6 N62 1.325(13) . ?
C6 N61 1.348(12) . ?
N11 C14 1.481(16) . ?
N11 C11 1.519(15) . ?
N12 C12 1.492(17) . ?
N12 C13 1.532(16) . ?
N21 C24 1.475(14) . ?
N21 C21 1.500(15) . ?
N22 C23 1.518(15) . ?
N22 C22 1.518(17) . ?
N31 C33 1.467(15) . ?
N31 C31 1.522(15) . ?
N32 C32 1.495(17) . ?
N32 C34 1.519(15) . ?
N41 C41 1.491(15) . ?
N41 C43 1.498(14) . ?
N42 C42 1.481(17) . ?
N42 C44 1.554(15) . ?
N51 C51 1.508(17) . ?
N51 C53 1.525(16) . ?
N52 C54 1.492(15) . ?
N52 C52 1.504(15) . ?
N61 C61 1.489(15) . ?
N61 C64 1.495(14) . ?
N62 C62 1.479(18) . ?
N62 C63 1.527(15) . ?
Cl1 O11 1.341(12) . ?
Cl1 O12 1.349(12) . ?
Cl1 O14 1.378(11) . ?
Cl1 O13 1.416(11) . ?
Cl2 O24 1.337(11) . ?
Cl2 O21 1.350(13) . ?
Cl2 O23 1.395(11) . ?
Cl2 O22 1.403(10) . ?
Cl3 O32 1.349(11) . ?
Cl3 O33 1.351(12) . ?
Cl3 O34 1.385(11) . ?
Cl3 O31 1.387(12) . ?
C43 C45 1.512(19) . ?
C53 C55 1.464(19) . ?
C13 C15 1.499(18) . ?
C63 C65 1.516(18) . ?
C23 C25 1.475(18) . ?
C34 C35 1.486(18) . ?
C44 C45 1.485(18) . ?
C64 C65 1.484(18) . ?
C54 C55 1.506(18) . ?
C24 C25 1.515(18) . ?
C14 C15 1.503(18) . ?
C33 C35 1.536(18) . ?
