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#$Date: 2016-03-23 00:49:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179130 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/92/4309253.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_4309253
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            'C52 H50 N4 Sb2'
_chemical_formula_weight         974.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.874(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9894(15)
_cell_length_b                   17.422(2)
_cell_length_c                   10.3495(13)
_cell_measurement_temperature    173(2)
_cell_volume                     2159.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13958
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.94
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0209
_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)+(0.0331P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0475
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                3921
_reflns_number_total             4965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050127vsi20050127_032156_2.cif
_cod_data_source_block           daltonm
_cod_database_code               4309253
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.592068(13) 0.025762(9) 0.112750(15) 0.01687(6) Uani 1 1 d . . .
N1 N 0.72094(18) 0.08566(14) 0.0405(2) 0.0243(5) Uani 1 1 d . . .
N2 N 0.42740(16) 0.02928(12) 0.0682(2) 0.0198(4) Uani 1 1 d . . .
C20 C 0.8315(2) 0.08270(17) 0.1090(3) 0.0280(6) Uani 1 1 d . . .
H20A H 0.8609 0.0296 0.1077 0.034 Uiso 1 1 calc R . .
H20B H 0.8250 0.0982 0.2004 0.034 Uiso 1 1 calc R . .
C21 C 0.9107(2) 0.13618(16) 0.0440(3) 0.0266(6) Uani 1 1 d . . .
C22 C 0.9237(2) 0.21203(19) 0.0819(3) 0.0404(8) Uani 1 1 d . . .
H22 H 0.8842 0.2308 0.1527 0.048 Uiso 1 1 calc R . .
C23 C 0.9937(3) 0.26088(19) 0.0179(4) 0.0493(9) Uani 1 1 d . . .
H23 H 1.0015 0.3128 0.0447 0.059 Uiso 1 1 calc R . .
C24 C 1.0519(3) 0.2343(2) -0.0846(4) 0.0459(9) Uani 1 1 d . . .
H24 H 1.0996 0.2678 -0.1287 0.055 Uiso 1 1 calc R . .
C25 C 1.0403(3) 0.1590(2) -0.1223(3) 0.0437(8) Uani 1 1 d . . .
H25 H 1.0812 0.1401 -0.1919 0.052 Uiso 1 1 calc R . .
C26 C 0.9694(2) 0.11056(18) -0.0592(3) 0.0347(7) Uani 1 1 d . . .
H26 H 0.9609 0.0589 -0.0874 0.042 Uiso 1 1 calc R . .
C1 C 0.5880(2) 0.10458(15) 0.2760(3) 0.0217(6) Uani 1 1 d . . .
C2 C 0.5306(2) 0.08391(17) 0.3841(3) 0.0279(6) Uani 1 1 d . . .
H2 H 0.4963 0.0348 0.3872 0.033 Uiso 1 1 calc R . .
C3 C 0.5227(2) 0.13403(19) 0.4878(3) 0.0353(7) Uani 1 1 d . . .
H3 H 0.4827 0.1194 0.5608 0.042 Uiso 1 1 calc R . .
C4 C 0.5732(3) 0.20523(19) 0.4844(3) 0.0409(8) Uani 1 1 d . . .
H4 H 0.5669 0.2398 0.5547 0.049 Uiso 1 1 calc R . .
C5 C 0.6327(3) 0.22638(18) 0.3796(3) 0.0382(8) Uani 1 1 d . . .
H5 H 0.6690 0.2748 0.3785 0.046 Uiso 1 1 calc R . .
C6 C 0.6392(2) 0.17655(16) 0.2758(3) 0.0281(6) Uani 1 1 d . . .
H6 H 0.6793 0.1917 0.2031 0.034 Uiso 1 1 calc R . .
C7 C 0.6475(2) -0.07371(15) 0.2183(2) 0.0208(5) Uani 1 1 d . . .
C12 C 0.7174(2) -0.06639(16) 0.3291(3) 0.0247(6) Uani 1 1 d . . .
H12 H 0.7407 -0.0169 0.3582 0.030 Uiso 1 1 calc R . .
C11 C 0.7530(2) -0.13120(17) 0.3971(3) 0.0310(7) Uani 1 1 d . . .
H11 H 0.8006 -0.1260 0.4727 0.037 Uiso 1 1 calc R . .
C10 C 0.7196(2) -0.20331(17) 0.3555(3) 0.0333(7) Uani 1 1 d . . .
H10 H 0.7444 -0.2475 0.4024 0.040 Uiso 1 1 calc R . .
C9 C 0.6500(2) -0.21117(17) 0.2453(3) 0.0315(7) Uani 1 1 d . . .
H9 H 0.6271 -0.2607 0.2163 0.038 Uiso 1 1 calc R . .
C8 C 0.6139(2) -0.14627(16) 0.1773(3) 0.0246(6) Uani 1 1 d . . .
H8 H 0.5658 -0.1516 0.1020 0.030 Uiso 1 1 calc R . .
C13 C 0.3433(2) 0.07876(16) 0.1228(2) 0.0224(5) Uani 1 1 d . . .
H13A H 0.2988 0.1026 0.0503 0.027 Uiso 1 1 calc R . .
H13B H 0.3825 0.1206 0.1713 0.027 Uiso 1 1 calc R . .
C14 C 0.2633(2) 0.04056(15) 0.2122(2) 0.0215(6) Uani 1 1 d . . .
C15 C 0.1607(2) 0.07556(17) 0.2310(3) 0.0258(6) Uani 1 1 d . . .
H15 H 0.1419 0.1218 0.1864 0.031 Uiso 1 1 calc R . .
C16 C 0.0859(2) 0.04380(18) 0.3137(3) 0.0318(7) Uani 1 1 d . . .
H16 H 0.0165 0.0684 0.3255 0.038 Uiso 1 1 calc R . .
C17 C 0.1118(2) -0.02347(19) 0.3790(3) 0.0357(7) Uani 1 1 d . . .
H17 H 0.0605 -0.0451 0.4357 0.043 Uiso 1 1 calc R . .
C18 C 0.2131(2) -0.05932(18) 0.3613(3) 0.0334(7) Uani 1 1 d . . .
H18 H 0.2314 -0.1056 0.4060 0.040 Uiso 1 1 calc R . .
C19 C 0.2881(2) -0.02729(17) 0.2779(3) 0.0274(6) Uani 1 1 d . . .
H19 H 0.3573 -0.0522 0.2658 0.033 Uiso 1 1 calc R . .
H1 H 0.729(2) 0.0728(18) -0.029(3) 0.025(9) 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'
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 N1 130.99(9) . . ?
N2 Sb1 N2 75.28(9) . 3_655 ?
N1 Sb1 N2 87.65(9) . 3_655 ?
N2 Sb1 C7 114.80(9) . . ?
N1 Sb1 C7 112.39(9) . . ?
N2 Sb1 C7 95.92(9) 3_655 . ?
N2 Sb1 C1 95.66(9) . . ?
N1 Sb1 C1 90.50(10) . . ?
N2 Sb1 C1 165.96(9) 3_655 . ?
C7 Sb1 C1 97.65(10) . . ?
N2 Sb1 Sb1 38.73(6) . 3_655 ?
N1 Sb1 Sb1 112.17(7) . 3_655 ?
N2 Sb1 Sb1 36.55(5) 3_655 3_655 ?
C7 Sb1 Sb1 108.97(7) . 3_655 ?
C1 Sb1 Sb1 133.50(6) . 3_655 ?
C20 N1 Sb1 119.10(18) . . ?
C13 N2 Sb1 128.28(16) . . ?
C13 N2 Sb1 124.35(15) . 3_655 ?
Sb1 N2 Sb1 104.72(9) . 3_655 ?
N1 C20 C21 109.5(2) . . ?
C26 C21 C22 118.2(3) . . ?
C26 C21 C20 120.0(3) . . ?
C22 C21 C20 121.8(3) . . ?
C21 C22 C23 120.8(3) . . ?
C24 C23 C22 120.2(3) . . ?
C25 C24 C23 119.4(3) . . ?
C24 C25 C26 120.3(3) . . ?
C21 C26 C25 121.1(3) . . ?
C2 C1 C6 118.0(3) . . ?
C2 C1 Sb1 119.47(19) . . ?
C6 C1 Sb1 122.5(2) . . ?
C1 C2 C3 120.9(3) . . ?
C4 C3 C2 119.8(3) . . ?
C5 C4 C3 120.3(3) . . ?
C4 C5 C6 119.6(3) . . ?
C5 C6 C1 121.3(3) . . ?
C8 C7 C12 119.3(2) . . ?
C8 C7 Sb1 120.30(19) . . ?
C12 C7 Sb1 120.39(19) . . ?
C11 C12 C7 120.0(3) . . ?
C10 C11 C12 120.4(3) . . ?
C11 C10 C9 120.0(3) . . ?
C10 C9 C8 119.7(3) . . ?
C7 C8 C9 120.5(3) . . ?
N2 C13 C14 116.5(2) . . ?
C19 C14 C15 118.2(2) . . ?
C19 C14 C13 123.0(2) . . ?
C15 C14 C13 118.8(2) . . ?
C16 C15 C14 120.9(3) . . ?
C17 C16 C15 120.3(3) . . ?
C16 C17 C18 119.7(3) . . ?
C17 C18 C19 119.9(3) . . ?
C14 C19 C18 121.0(3) . . ?
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 2.0057(19) . ?
Sb1 N1 2.038(2) . ?
Sb1 N2 2.107(2) 3_655 ?
Sb1 C7 2.137(3) . ?
Sb1 C1 2.180(3) . ?
Sb1 Sb1 3.2573(4) 3_655 ?
N1 C20 1.473(3) . ?
N2 C13 1.461(3) . ?
N2 Sb1 2.107(2) 3_655 ?
C20 C21 1.512(4) . ?
C21 C26 1.383(4) . ?
C21 C22 1.385(4) . ?
C22 C23 1.387(4) . ?
C23 C24 1.379(5) . ?
C24 C25 1.375(5) . ?
C25 C26 1.385(4) . ?
C1 C2 1.390(4) . ?
C1 C6 1.396(4) . ?
C2 C3 1.390(4) . ?
C3 C4 1.381(5) . ?
C4 C5 1.378(5) . ?
C5 C6 1.387(4) . ?
C7 C8 1.387(4) . ?
C7 C12 1.392(4) . ?
C12 C11 1.386(4) . ?
C11 C10 1.381(4) . ?
C10 C9 1.386(4) . ?
C9 C8 1.390(4) . ?
C13 C14 1.520(4) . ?
C14 C19 1.389(4) . ?
C14 C15 1.394(3) . ?
C15 C16 1.386(4) . ?
C16 C17 1.380(4) . ?
C17 C18 1.386(4) . ?
C18 C19 1.394(4) . ?
