#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:49:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179130 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/92/4309252.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_4309252
loop_
_publ_author_name
'May C. Copsey'
'Sabrina B. Gallon'
'Sara K. Grocott'
'John C. Jeffery'
'Christopher A. Russell'
'John M. Slattery'
_publ_section_title
;
Synthetic and Structural Studies of Cyclodistib(V)azanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5495
_journal_page_last               5500
_journal_paper_doi               10.1021/ic050127v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C25 H22 Bi0 N Sb'
_chemical_formula_weight         458.19
_chemical_name_systematic
; 
 ? 
;
_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                70.90(3)
_cell_angle_beta                 74.33(3)
_cell_angle_gamma                71.59(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0485(18)
_cell_length_b                   10.702(2)
_cell_length_c                   11.459(2)
_cell_measurement_temperature    293(2)
_cell_volume                     977.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11047
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.420
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.87
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0245P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0479
_reflns_number_gt                4089
_reflns_number_total             4473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050127vsi20050127_032156_1.cif
_cod_data_source_block           sunnym
_cod_original_cell_volume        977.5(3)
_cod_database_code               4309252
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
Sb1 Sb 0.926476(15) 0.873880(12) 0.097191(12) 0.01316(5) Uani 1 1 d . . .
C20 C 0.7414(2) 0.85597(18) 0.26721(19) 0.0167(4) Uani 1 1 d . . .
C21 C 0.7686(3) 0.8565(2) 0.3815(2) 0.0217(4) Uani 1 1 d . . .
H21 H 0.8664 0.8649 0.3850 0.026 Uiso 1 1 calc R . .
C22 C 0.6530(3) 0.8448(2) 0.4899(2) 0.0269(5) Uani 1 1 d . . .
H22 H 0.6737 0.8458 0.5647 0.032 Uiso 1 1 calc R . .
C23 C 0.5075(3) 0.8318(2) 0.4864(2) 0.0292(5) Uani 1 1 d . . .
H23 H 0.4293 0.8252 0.5585 0.035 Uiso 1 1 calc R . .
C24 C 0.4788(3) 0.8285(2) 0.3752(2) 0.0306(5) Uani 1 1 d . . .
H24 H 0.3816 0.8180 0.3729 0.037 Uiso 1 1 calc R . .
C25 C 0.5946(2) 0.8409(2) 0.2666(2) 0.0227(4) Uani 1 1 d . . .
H25 H 0.5733 0.8391 0.1923 0.027 Uiso 1 1 calc R . .
C26 C 1.1035(2) 0.71856(18) 0.19194(18) 0.0156(4) Uani 1 1 d . . .
C27 C 1.0613(2) 0.60745(19) 0.28724(19) 0.0180(4) Uani 1 1 d . . .
H27 H 0.9572 0.6000 0.3068 0.022 Uiso 1 1 calc R . .
C28 C 1.1732(3) 0.5085(2) 0.3526(2) 0.0213(4) Uani 1 1 d . . .
H28 H 1.1442 0.4348 0.4153 0.026 Uiso 1 1 calc R . .
C29 C 1.3276(3) 0.5192(2) 0.3248(2) 0.0213(4) Uani 1 1 d . . .
H29 H 1.4023 0.4535 0.3696 0.026 Uiso 1 1 calc R . .
C30 C 1.3714(2) 0.6283(2) 0.2297(2) 0.0213(4) Uani 1 1 d . . .
H30 H 1.4756 0.6352 0.2105 0.026 Uiso 1 1 calc R . .
C31 C 1.2598(2) 0.72699(19) 0.16349(19) 0.0186(4) Uani 1 1 d . . .
H31 H 1.2900 0.7993 0.0995 0.022 Uiso 1 1 calc R . .
C32 C 0.8165(2) 0.79348(19) 0.00529(19) 0.0162(4) Uani 1 1 d . . .
C33 C 0.8425(3) 0.6542(2) 0.0256(2) 0.0239(5) Uani 1 1 d . . .
H33 H 0.9102 0.5941 0.0794 0.029 Uiso 1 1 calc R . .
C34 C 0.7684(3) 0.6032(2) -0.0336(2) 0.0279(5) Uani 1 1 d . . .
H34 H 0.7877 0.5094 -0.0201 0.034 Uiso 1 1 calc R . .
C35 C 0.6662(3) 0.6915(2) -0.1124(2) 0.0262(5) Uani 1 1 d . . .
H35 H 0.6167 0.6574 -0.1522 0.031 Uiso 1 1 calc R . .
C36 C 0.6381(3) 0.8298(2) -0.1318(2) 0.0296(5) Uani 1 1 d . . .
H36 H 0.5680 0.8894 -0.1838 0.036 Uiso 1 1 calc R . .
C37 C 0.7133(3) 0.8812(2) -0.0746(2) 0.0259(5) Uani 1 1 d . . .
H37 H 0.6947 0.9751 -0.0895 0.031 Uiso 1 1 calc R . .
C47 C 0.7848(2) 1.16462(19) 0.13588(19) 0.0176(4) Uani 1 1 d . . .
H47A H 0.6991 1.1209 0.1809 0.021 Uiso 1 1 calc R . .
H47B H 0.7419 1.2462 0.0743 0.021 Uiso 1 1 calc R . .
C48 C 0.8356(2) 1.20859(19) 0.22879(19) 0.0175(4) Uani 1 1 d . . .
C49 C 0.9553(3) 1.1261(2) 0.2944(2) 0.0236(5) Uani 1 1 d . . .
H49 H 1.0141 1.0440 0.2761 0.028 Uiso 1 1 calc R . .
C50 C 0.9882(3) 1.1646(2) 0.3866(2) 0.0309(5) Uani 1 1 d . . .
H50 H 1.0689 1.1082 0.4299 0.037 Uiso 1 1 calc R . .
C51 C 0.9016(3) 1.2869(2) 0.4150(2) 0.0314(5) Uani 1 1 d . . .
H51 H 0.9226 1.3116 0.4783 0.038 Uiso 1 1 calc R . .
C52 C 0.7848(3) 1.3714(2) 0.3492(2) 0.0302(5) Uani 1 1 d . . .
H52 H 0.7275 1.4541 0.3669 0.036 Uiso 1 1 calc R . .
C53 C 0.7525(3) 1.3327(2) 0.2561(2) 0.0230(5) Uani 1 1 d . . .
H53 H 0.6741 1.3908 0.2112 0.028 Uiso 1 1 calc R . .
N2 N 0.90519(19) 1.07250(15) 0.06834(15) 0.0154(3) 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
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sb Sb -0.5866 1.5461 '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
N2 Sb1 N2 74.67(8) . 2_775 ?
N2 Sb1 C32 124.38(7) . . ?
N2 Sb1 C32 92.45(7) 2_775 . ?
N2 Sb1 C26 122.40(7) . . ?
N2 Sb1 C26 92.78(7) 2_775 . ?
C32 Sb1 C26 111.89(7) . . ?
N2 Sb1 C20 95.46(8) . . ?
N2 Sb1 C20 170.12(6) 2_775 . ?
C32 Sb1 C20 92.87(8) . . ?
C26 Sb1 C20 92.96(8) . . ?
N2 Sb1 Sb1 38.74(5) . 2_775 ?
N2 Sb1 Sb1 35.93(4) 2_775 2_775 ?
C32 Sb1 Sb1 111.80(6) . 2_775 ?
C26 Sb1 Sb1 110.95(6) . 2_775 ?
C20 Sb1 Sb1 134.20(5) . 2_775 ?
C25 C20 C21 117.3(2) . . ?
C25 C20 Sb1 121.79(16) . . ?
C21 C20 Sb1 120.90(15) . . ?
C22 C21 C20 121.6(2) . . ?
C23 C22 C21 120.0(2) . . ?
C22 C23 C24 119.5(2) . . ?
C23 C24 C25 120.4(2) . . ?
C20 C25 C24 121.2(2) . . ?
C31 C26 C27 118.75(18) . . ?
C31 C26 Sb1 121.38(14) . . ?
C27 C26 Sb1 119.84(14) . . ?
C28 C27 C26 120.58(19) . . ?
C29 C28 C27 120.12(19) . . ?
C28 C29 C30 119.87(19) . . ?
C31 C30 C29 120.14(19) . . ?
C30 C31 C26 120.52(19) . . ?
C33 C32 C37 118.60(18) . . ?
C33 C32 Sb1 121.21(15) . . ?
C37 C32 Sb1 120.17(14) . . ?
C32 C33 C34 120.6(2) . . ?
C35 C34 C33 120.1(2) . . ?
C36 C35 C34 119.7(2) . . ?
C35 C36 C37 120.5(2) . . ?
C36 C37 C32 120.54(19) . . ?
N2 C47 C48 117.35(17) . . ?
C49 C48 C53 118.18(19) . . ?
C49 C48 C47 122.53(18) . . ?
C53 C48 C47 119.16(18) . . ?
C50 C49 C48 120.7(2) . . ?
C49 C50 C51 120.3(2) . . ?
C52 C51 C50 119.8(2) . . ?
C51 C52 C53 119.7(2) . . ?
C52 C53 C48 121.2(2) . . ?
C47 N2 Sb1 126.94(13) . . ?
C47 N2 Sb1 127.22(12) . 2_775 ?
Sb1 N2 Sb1 105.33(8) . 2_775 ?
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
Sb1 N2 1.9951(16) . ?
Sb1 N2 2.1276(18) 2_775 ?
Sb1 C32 2.131(2) . ?
Sb1 C26 2.141(2) . ?
Sb1 C20 2.199(2) . ?
Sb1 Sb1 3.2789(13) 2_775 ?
C20 C25 1.389(3) . ?
C20 C21 1.398(3) . ?
C21 C22 1.390(3) . ?
C22 C23 1.379(3) . ?
C23 C24 1.380(3) . ?
C24 C25 1.393(3) . ?
C26 C31 1.388(3) . ?
C26 C27 1.401(3) . ?
C27 C28 1.386(3) . ?
C28 C29 1.379(3) . ?
C29 C30 1.391(3) . ?
C30 C31 1.388(3) . ?
C32 C33 1.383(3) . ?
C32 C37 1.391(3) . ?
C33 C34 1.387(3) . ?
C34 C35 1.380(3) . ?
C35 C36 1.372(3) . ?
C36 C37 1.381(3) . ?
C47 N2 1.457(2) . ?
C47 C48 1.515(3) . ?
C48 C49 1.385(3) . ?
C48 C53 1.394(3) . ?
C49 C50 1.382(3) . ?
C50 C51 1.388(3) . ?
C51 C52 1.372(4) . ?
C52 C53 1.388(3) . ?
N2 Sb1 2.1276(18) 2_775 ?
