#------------------------------------------------------------------------------
#$Date: 2019-11-25 02:28:46 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239969 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/06/4350620.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_4350620
loop_
_publ_author_name
'Eisler, Dana J.'
'Chivers, Tristram'
_publ_section_title
;
 Bis(1 degree-amino)cyclodistib(III)azanes: the first structural
 characterization of cis and trans isomers of a single
 cyclodipnict(III)azane.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10734
_journal_page_last               10742
_journal_paper_doi               10.1021/ic061660t
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C32 H54 N4 Sb2'
_chemical_formula_sum            'C32 H54 N4 Sb2'
_chemical_formula_weight         738.29
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.10(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.111(2)
_cell_length_b                   9.3393(19)
_cell_length_c                   15.749(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1735.0(6)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phiω 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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15157
_diffrn_reflns_theta_full        24.89
_diffrn_reflns_theta_max         24.89
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_T_max  0.9541
_exptl_absorpt_correction_T_min  0.8579
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2993
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0354
_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)+(0.0463P)²+2.0152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                2429
_reflns_number_total             2993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061660tsi20060901_013006.cif
_cod_data_source_block           trans-3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4350620
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Sb1 Sb 0.02460(2) 0.04160(3) 0.908847(16) 0.03096(13) Uani 1 1 d .
N1 N -0.1007(3) 0.0485(4) 0.9746(2) 0.0323(8) Uani 1 1 d .
C1 C -0.2243(4) 0.0651(4) 0.9395(3) 0.0336(10) Uani 1 1 d .
C2 C -0.2740(4) 0.1456(5) 1.0069(3) 0.0425(11) Uani 1 1 d .
H2A H -0.2426 0.2426 1.0143 0.064 Uiso 1 1 calc R
H2B H -0.2548 0.0948 1.0627 0.064 Uiso 1 1 calc R
H2C H -0.3567 0.1508 0.9867 0.064 Uiso 1 1 calc R
C3 C -0.2446(4) 0.1478(5) 0.8549(3) 0.0438(11) Uani 1 1 d .
H3A H -0.2074 0.2414 0.8652 0.066 Uiso 1 1 calc R
H3B H -0.3263 0.1613 0.8325 0.066 Uiso 1 1 calc R
H3C H -0.2134 0.0943 0.8122 0.066 Uiso 1 1 calc R
C4 C -0.2822(4) -0.0833(5) 0.9230(3) 0.0482(12) Uani 1 1 d .
H4A H -0.2521 -0.1350 0.8790 0.072 Uiso 1 1 calc R
H4B H -0.3642 -0.0706 0.9021 0.072 Uiso 1 1 calc R
H4C H -0.2669 -0.1383 0.9774 0.072 Uiso 1 1 calc R
N2 N -0.0333(3) -0.1406(4) 0.8389(2) 0.0327(8) Uani 1 1 d D
H2D H -0.058(4) -0.202(4) 0.877(2) 0.039 Uiso 1 1 d D
C5 C 0.0198(3) -0.2051(4) 0.7770(2) 0.0302(9) Uani 1 1 d .
C6 C 0.0257(4) -0.1297(5) 0.7010(3) 0.0325(9) Uani 1 1 d .
C7 C 0.0751(4) -0.1968(5) 0.6401(3) 0.0439(11) Uani 1 1 d .
H7A H 0.0813 -0.1462 0.5890 0.053 Uiso 1 1 calc R
C8 C 0.1151(4) -0.3349(5) 0.6520(3) 0.0491(13) Uani 1 1 d .
H8A H 0.1478 -0.3792 0.6092 0.059 Uiso 1 1 calc R
C9 C 0.1077(4) -0.4085(5) 0.7259(3) 0.0446(12) Uani 1 1 d .
H9A H 0.1343 -0.5044 0.7330 0.054 Uiso 1 1 calc R
C10 C 0.0626(4) -0.3468(4) 0.7903(3) 0.0345(10) Uani 1 1 d .
C11 C -0.1191(5) 0.0199(6) 0.5973(3) 0.0501(13) Uani 1 1 d .
H11A H -0.1502 0.1168 0.5863 0.075 Uiso 1 1 calc R
H11B H -0.1793 -0.0458 0.6047 0.075 Uiso 1 1 calc R
H11C H -0.0887 -0.0114 0.5478 0.075 Uiso 1 1 calc R
C12 C -0.0241(4) 0.0200(5) 0.6803(3) 0.0360(10) Uani 1 1 d .
H12A H -0.0585 0.0494 0.7296 0.043 Uiso 1 1 calc R
C13 C 0.0649(5) 0.1316(5) 0.6727(4) 0.0541(13) Uani 1 1 d .
H13A H 0.1276 0.1269 0.7244 0.081 Uiso 1 1 calc R
H13B H 0.0307 0.2272 0.6684 0.081 Uiso 1 1 calc R
H13C H 0.0937 0.1124 0.6205 0.081 Uiso 1 1 calc R
C14 C 0.1460(5) -0.5443(5) 0.8981(4) 0.0501(13) Uani 1 1 d .
H14A H 0.2209 -0.4995 0.9062 0.075 Uiso 1 1 calc R
H14B H 0.1376 -0.6175 0.8525 0.075 Uiso 1 1 calc R
H14C H 0.1386 -0.5888 0.9528 0.075 Uiso 1 1 calc R
C15 C 0.0540(4) -0.4303(5) 0.8711(3) 0.0374(10) Uani 1 1 d .
H15A H 0.0625 -0.3604 0.9202 0.045 Uiso 1 1 calc R
C16 C -0.0626(5) -0.4995(6) 0.8595(3) 0.0496(13) Uani 1 1 d .
H16A H -0.1213 -0.4255 0.8457 0.074 Uiso 1 1 calc R
H16B H -0.0679 -0.5482 0.9135 0.074 Uiso 1 1 calc R
H16C H -0.0735 -0.5692 0.8118 0.074 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
N1 Sb1 N1 77.90(15) . 3_557
N1 Sb1 N2 95.53(14) . .
N1 Sb1 N2 99.76(13) 3_557 .
C1 N1 Sb1 128.6(3) . .
C1 N1 Sb1 126.2(3) . 3_557
Sb1 N1 Sb1 102.10(15) . 3_557
N1 C1 C3 109.3(4) . .
N1 C1 C2 108.4(3) . .
C3 C1 C2 110.4(4) . .
N1 C1 C4 110.5(3) . .
C3 C1 C4 109.4(4) . .
C2 C1 C4 108.8(4) . .
C5 N2 Sb1 124.5(3) . .
C6 C5 N2 119.5(4) . .
C6 C5 C10 120.4(4) . .
N2 C5 C10 120.1(4) . .
C7 C6 C5 118.4(4) . .
C7 C6 C12 118.4(4) . .
C5 C6 C12 123.2(4) . .
C8 C7 C6 121.4(4) . .
C9 C8 C7 119.8(4) . .
C8 C9 C10 121.8(4) . .
C9 C10 C5 118.2(4) . .
C9 C10 C15 121.0(4) . .
C5 C10 C15 120.7(4) . .
C13 C12 C6 113.0(4) . .
C13 C12 C11 110.0(4) . .
C6 C12 C11 111.5(4) . .
C10 C15 C16 110.8(4) . .
C10 C15 C14 114.0(4) . .
C16 C15 C14 109.6(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 N1 2.022(4) .
Sb1 N1 2.039(3) 3_557
Sb1 N2 2.061(3) .
N1 C1 1.482(5) .
N1 Sb1 2.039(3) 3_557
C1 C3 1.511(6) .
C1 C2 1.531(6) .
C1 C4 1.548(6) .
N2 C5 1.418(5) .
C5 C6 1.404(6) .
C5 C10 1.419(6) .
C6 C7 1.390(6) .
C6 C12 1.528(6) .
C7 C8 1.376(7) .
C8 C9 1.372(7) .
C9 C10 1.382(6) .
C10 C15 1.516(6) .
C11 C12 1.533(6) .
C12 C13 1.524(7) .
C14 C15 1.530(7) .
C15 C16 1.526(7) .
