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#$Date: 2016-03-25 12:15:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179806 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/02/7010213.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_7010213
loop_
_publ_author_name
'Bryant, Richard'
'James, Siân C.'
'Jeffery, John C.'
'Norman, Nicholas C.'
'Orpen, A. Guy'
'Weckenmann, Ulrike'
_publ_section_title
;
 Antimony imido and imido--amido compounds: a new route to an
 imidoantimony macrocycle
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4007
_journal_paper_doi               10.1039/b007020n
_journal_year                    2000
_chemical_formula_sum            'C32 H38 N4 Sb2'
_chemical_formula_weight         722.16
_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                101.00(2)
_cell_angle_beta                 110.705(14)
_cell_angle_gamma                107.892(14)
_cell_formula_units_Z            1
_cell_length_a                   7.9276(19)
_cell_length_b                   10.012(3)
_cell_length_c                   11.075(4)
_cell_measurement_temperature    173(2)
_cell_volume                     736.9(4)
_computing_cell_refinement       SMART
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3491
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.860
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0085P)²+3.0598P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                2252
_reflns_number_total             2479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007020n.txt
_cod_data_source_block           reedd
_cod_original_sg_symbol_H-M      P1(bar)
_cod_database_code               7010213
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 -0.13891(5) 0.08543(4) -0.04460(3) 0.02398(11) Uani 1 1 d . . .
N1 N 0.0658(7) 0.2649(5) -0.0492(5) 0.0304(10) Uani 1 1 d . . .
H1 H 0.165(8) 0.283(5) 0.017(5) 0.022(14) Uiso 1 1 d . . .
N2 N 0.0649(6) 0.0782(4) 0.1254(4) 0.0239(9) Uani 1 1 d . . .
C11 C 0.0624(7) 0.3671(5) -0.1198(5) 0.0254(10) Uani 1 1 d . . .
C12 C 0.2150(8) 0.5119(5) -0.0558(5) 0.0313(12) Uani 1 1 d . . .
C13 C 0.2218(9) 0.6104(6) -0.1296(7) 0.0415(14) Uani 1 1 d . . .
H13 H 0.3257 0.7073 -0.0873 0.050 Uiso 1 1 calc R . .
C14 C 0.0819(9) 0.5707(7) -0.2621(7) 0.0448(15) Uani 1 1 d . . .
H14 H 0.0891 0.6392 -0.3107 0.054 Uiso 1 1 calc R . .
C15 C -0.0700(8) 0.4287(6) -0.3235(6) 0.0372(13) Uani 1 1 d . . .
H15 H -0.1674 0.4013 -0.4146 0.045 Uiso 1 1 calc R . .
C16 C -0.0830(7) 0.3262(6) -0.2553(5) 0.0294(11) Uani 1 1 d . . .
C17 C -0.2504(8) 0.1730(6) -0.3264(5) 0.0390(13) Uani 1 1 d . . .
H17A H -0.3394 0.1628 -0.2827 0.059 Uiso 1 1 calc R . .
H17B H -0.1967 0.0972 -0.3196 0.059 Uiso 1 1 calc R . .
H17C H -0.3236 0.1595 -0.4232 0.059 Uiso 1 1 calc R . .
C18 C 0.3665(8) 0.5599(6) 0.0895(6) 0.0380(13) Uani 1 1 d . . .
H18A H 0.4411 0.4974 0.0961 0.057 Uiso 1 1 calc R . .
H18B H 0.3005 0.5494 0.1492 0.057 Uiso 1 1 calc R . .
H18C H 0.4571 0.6643 0.1180 0.057 Uiso 1 1 calc R . .
C21 C 0.1121(7) 0.1405(5) 0.2663(5) 0.0218(10) Uani 1 1 d . . .
C22 C -0.0309(7) 0.0990(5) 0.3148(5) 0.0282(11) Uani 1 1 d . . .
C23 C 0.0232(8) 0.1635(6) 0.4526(5) 0.0326(12) Uani 1 1 d . . .
H23 H -0.0725 0.1358 0.4864 0.039 Uiso 1 1 calc R . .
C24 C 0.2121(8) 0.2666(6) 0.5421(5) 0.0376(13) Uani 1 1 d . . .
H24 H 0.2453 0.3108 0.6358 0.045 Uiso 1 1 calc R . .
C25 C 0.3519(8) 0.3047(6) 0.4939(5) 0.0340(12) Uani 1 1 d . . .
H25 H 0.4823 0.3750 0.5559 0.041 Uiso 1 1 calc R . .
C26 C 0.3077(7) 0.2436(5) 0.3578(5) 0.0270(11) Uani 1 1 d . . .
C27 C 0.4642(7) 0.2851(6) 0.3092(5) 0.0364(13) Uani 1 1 d . . .
H27A H 0.4118 0.3052 0.2234 0.055 Uiso 1 1 calc R . .
H27B H 0.5049 0.2029 0.2937 0.055 Uiso 1 1 calc R . .
H27C H 0.5784 0.3746 0.3788 0.055 Uiso 1 1 calc R . .
C28 C -0.2390(8) -0.0140(6) 0.2215(6) 0.0410(14) Uani 1 1 d . . .
H28A H -0.2357 -0.1021 0.1675 0.061 Uiso 1 1 calc R . .
H28B H -0.3089 0.0296 0.1597 0.061 Uiso 1 1 calc R . .
H28C H -0.3078 -0.0430 0.2766 0.061 Uiso 1 1 calc R . .
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 92.16(17) . . ?
N2 Sb1 N2 77.49(16) . 2 ?
N1 Sb1 N2 98.76(17) . 2 ?
N2 Sb1 Sb1 39.01(10) . 2 ?
N1 Sb1 Sb1 97.02(13) . 2 ?
N2 Sb1 Sb1 38.47(11) 2 2 ?
C11 N1 Sb1 136.2(4) . . ?
C21 N2 Sb1 129.7(3) . . ?
C21 N2 Sb1 126.2(3) . 2 ?
Sb1 N2 Sb1 102.51(16) . 2 ?
N1 C11 C12 118.6(4) . . ?
N1 C11 C16 121.7(4) . . ?
C12 C11 C16 119.6(4) . . ?
C13 C12 C11 118.9(5) . . ?
C13 C12 C18 120.4(5) . . ?
C11 C12 C18 120.6(5) . . ?
C14 C13 C12 121.7(5) . . ?
C13 C14 C15 119.0(5) . . ?
C16 C15 C14 121.7(5) . . ?
C15 C16 C11 119.1(5) . . ?
C15 C16 C17 119.8(5) . . ?
C11 C16 C17 121.1(4) . . ?
C22 C21 C26 120.2(4) . . ?
C22 C21 N2 121.1(4) . . ?
C26 C21 N2 118.7(4) . . ?
C23 C22 C21 118.5(5) . . ?
C23 C22 C28 119.7(5) . . ?
C21 C22 C28 121.8(4) . . ?
C24 C23 C22 121.8(5) . . ?
C25 C24 C23 119.2(5) . . ?
C24 C25 C26 121.8(5) . . ?
C25 C26 C21 118.4(5) . . ?
C25 C26 C27 120.5(4) . . ?
C21 C26 C27 121.0(4) . . ?
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 2.033(4) . ?
Sb1 N1 2.042(4) . ?
Sb1 N2 2.057(4) 2 ?
Sb1 Sb1 3.1898(10) 2 ?
N1 C11 1.403(6) . ?
N2 C21 1.427(6) . ?
N2 Sb1 2.057(4) 2 ?
C11 C12 1.411(7) . ?
C11 C16 1.414(7) . ?
C12 C13 1.396(7) . ?
C12 C18 1.499(8) . ?
C13 C14 1.377(9) . ?
C14 C15 1.391(8) . ?
C15 C16 1.386(7) . ?
C16 C17 1.511(7) . ?
C21 C22 1.404(7) . ?
C21 C26 1.415(6) . ?
C22 C23 1.387(7) . ?
C22 C28 1.507(7) . ?
C23 C24 1.378(8) . ?
C24 C25 1.376(7) . ?
C25 C26 1.384(7) . ?
C26 C27 1.497(7) . ?
