#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:56:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179944 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/39/7023985.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_7023985
loop_
_publ_author_name
'Fridrichová, Adéla'
'Mairychová, Barbora'
'Padělková, Zdeňka'
'Lyčka, Antonín'
'Jurkschat, Klaus'
'Jambor, Roman'
'Dostál, Libor'
_publ_section_title
;
 Straightforward synthesis of novel cyclic metallasiloxanes supported by
 an N,C,N-chelating ligand.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16403
_journal_page_last               16411
_journal_paper_doi               10.1039/c3dt52230j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C48 H58 N4 O4 Sb2 Si2'
_chemical_formula_sum            'C48 H58 N4 O4 Sb2 Si2'
_chemical_formula_weight         1054.66
_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
_cell_angle_beta                 113.078(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7080(5)
_cell_length_b                   15.9991(10)
_cell_length_c                   13.7490(6)
_cell_measurement_reflns_used    20112
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2369.3(2)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20039
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0291
_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)+(0.0192P)²+2.7364P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                4424
_reflns_number_total             5376
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52230j.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7023985
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
Sb1 Sb -0.053802(15) -0.044561(10) 0.292794(13) 0.01754(6) Uani 1 1 d .
Si1 Si -0.18451(6) 0.02079(4) 0.45540(6) 0.01804(15) Uani 1 1 d .
C13 C -0.2379(2) -0.08992(17) 0.4551(2) 0.0224(6) Uani 1 1 d .
O2 O 0.09615(17) -0.04774(12) 0.42645(14) 0.0221(4) Uani 1 1 d .
O1 O -0.12614(16) 0.03380(11) 0.36748(14) 0.0205(4) Uani 1 1 d .
N2 N -0.2524(2) 0.03016(14) 0.13542(18) 0.0236(5) Uani 1 1 d .
C1 C 0.0068(2) 0.05719(15) 0.22046(19) 0.0175(5) Uani 1 1 d .
N1 N 0.1375(2) -0.09426(14) 0.23703(18) 0.0227(5) Uani 1 1 d .
C14 C -0.1705(3) -0.14531(17) 0.5368(2) 0.0243(6) Uani 1 1 d .
H14 H -0.0957 -0.1280 0.5889 0.029 Uiso 1 1 d R
C4 C 0.0905(3) 0.19394(18) 0.1407(2) 0.0289(6) Uani 1 1 d .
H4 H 0.1203 0.2413 0.1192 0.035 Uiso 1 1 d R
C5 C -0.0313(3) 0.19047(17) 0.1308(2) 0.0248(6) Uani 1 1 d .
H5 H -0.0853 0.2340 0.0977 0.030 Uiso 1 1 d R
C9 C 0.2132(3) -0.16430(18) 0.2952(2) 0.0312(7) Uani 1 1 d .
H9A H 0.2857 -0.1686 0.2791 0.037 Uiso 1 1 d R
H9B H 0.1660 -0.2150 0.2749 0.037 Uiso 1 1 d R
H9C H 0.2379 -0.1554 0.3697 0.037 Uiso 1 1 d R
C11 C -0.2594(3) 0.0005(2) 0.0330(2) 0.0356(7) Uani 1 1 d .
H11A H -0.2810 -0.0578 0.0257 0.043 Uiso 1 1 d R
H11B H -0.1805 0.0079 0.0281 0.043 Uiso 1 1 d R
H11C H -0.3216 0.0316 -0.0222 0.043 Uiso 1 1 d R
C7 C 0.2100(2) -0.01680(17) 0.2637(2) 0.0232(6) Uani 1 1 d .
H7A H 0.2721 -0.0180 0.2333 0.028 Uiso 1 1 d R
H7B H 0.2527 -0.0124 0.3398 0.028 Uiso 1 1 d R
C3 C 0.1682(3) 0.12664(18) 0.1831(2) 0.0261(6) Uani 1 1 d .
H3 H 0.2487 0.1274 0.1855 0.031 Uiso 1 1 d R
C6 C -0.0742(2) 0.12204(17) 0.1700(2) 0.0208(5) Uani 1 1 d .
C2 C 0.1274(2) 0.05775(16) 0.2220(2) 0.0207(6) Uani 1 1 d .
C8 C 0.0889(3) -0.11132(19) 0.1233(2) 0.0302(6) Uani 1 1 d .
H8A H 0.0415 -0.0642 0.0852 0.036 Uiso 1 1 d R
H8B H 0.0366 -0.1599 0.1079 0.036 Uiso 1 1 d R
H8C H 0.1568 -0.1211 0.1022 0.036 Uiso 1 1 d R
C24 C -0.2993(3) 0.17833(17) 0.3993(2) 0.0238(6) Uani 1 1 d .
H24 H -0.2243 0.1932 0.3956 0.029 Uiso 1 1 d R
C23 C -0.3890(3) 0.23868(19) 0.3835(2) 0.0293(6) Uani 1 1 d .
H23 H -0.3732 0.2937 0.3707 0.035 Uiso 1 1 d R
C21 C -0.5237(3) 0.13609(19) 0.4077(2) 0.0304(7) Uani 1 1 d .
H21 H -0.5988 0.1215 0.4113 0.037 Uiso 1 1 d R
C20 C -0.4332(3) 0.07580(18) 0.4236(2) 0.0247(6) Uani 1 1 d .
H20 H -0.4494 0.0209 0.4366 0.030 Uiso 1 1 d R
C22 C -0.5024(3) 0.21716(19) 0.3873(2) 0.0323(7) Uani 1 1 d .
H22 H -0.5635 0.2576 0.3757 0.039 Uiso 1 1 d R
C15 C -0.2128(3) -0.22586(18) 0.5408(2) 0.0295(6) Uani 1 1 d .
H15 H -0.1676 -0.2612 0.5963 0.035 Uiso 1 1 d R
C19 C -0.3187(2) 0.09514(17) 0.41989(19) 0.0195(5) Uani 1 1 d .
C10 C -0.2087(2) 0.11668(17) 0.1546(2) 0.0233(6) Uani 1 1 d .
H10A H -0.2185 0.1376 0.2171 0.028 Uiso 1 1 d R
H10B H -0.2584 0.1512 0.0951 0.028 Uiso 1 1 d R
C18 C -0.3473(3) -0.12081(19) 0.3773(2) 0.0281(6) Uani 1 1 d .
H18 H -0.3935 -0.0862 0.3213 0.034 Uiso 1 1 d R
C16 C -0.3218(3) -0.25322(18) 0.4635(3) 0.0329(7) Uani 1 1 d .
H16 H -0.3503 -0.3069 0.4671 0.039 Uiso 1 1 d R
C12 C -0.3724(3) 0.0220(2) 0.1430(2) 0.0345(7) Uani 1 1 d .
H12A H -0.4324 0.0563 0.0902 0.041 Uiso 1 1 d R
H12B H -0.3655 0.0396 0.2119 0.041 Uiso 1 1 d R
H12C H -0.3985 -0.0353 0.1321 0.041 Uiso 1 1 d R
C17 C -0.3888(3) -0.20091(19) 0.3807(3) 0.0335(7) Uani 1 1 d .
H17 H -0.4617 -0.2197 0.3275 0.040 Uiso 1 1 d 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'
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'
Si Si 0.0817 0.0704 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -1 0.034
0 -1 1 0.115
0 1 1 0.113
0 -1 -1 0.161
1 0 0 0.011
-1 0 0 0.086
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
O2 Sb1 O1 86.55(7) .
O2 Sb1 C1 96.57(9) .
O1 Sb1 C1 92.59(8) .
O2 Si1 O1 115.34(10) 3_556
O2 Si1 C19 103.57(11) 3_556
O1 Si1 C19 106.25(10) .
O2 Si1 C13 109.71(11) 3_556
O1 Si1 C13 110.95(10) .
C19 Si1 C13 110.69(12) .
C18 C13 C14 116.6(3) .
C18 C13 Si1 122.6(2) .
C14 C13 Si1 120.8(2) .
Si1 O2 Sb1 156.35(12) 3_556
Si1 O1 Sb1 133.51(11) .
C12 N2 C11 110.5(2) .
C12 N2 C10 110.6(2) .
C11 N2 C10 111.5(2) .
C6 C1 C2 119.1(2) .
C6 C1 Sb1 120.44(18) .
C2 C1 Sb1 120.41(18) .
C9 N1 C7 110.2(2) .
C9 N1 C8 109.9(2) .
C7 N1 C8 111.6(2) .
C15 C14 C13 121.3(3) .
C15 C14 H14 119.2 .
C13 C14 H14 119.5 .
C5 C4 C3 119.6(3) .
C5 C4 H4 120.2 .
C3 C4 H4 120.2 .
C4 C5 C6 120.5(3) .
C4 C5 H5 119.7 .
C6 C5 H5 119.8 .
N1 C9 H9A 109.3 .
N1 C9 H9B 109.4 .
H9A C9 H9B 109.5 .
N1 C9 H9C 109.6 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
N2 C11 H11A 109.3 .
N2 C11 H11B 109.7 .
H11A C11 H11B 109.5 .
N2 C11 H11C 109.4 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
N1 C7 C2 110.7(2) .
N1 C7 H7A 109.5 .
C2 C7 H7A 109.4 .
N1 C7 H7B 109.5 .
C2 C7 H7B 109.6 .
H7A C7 H7B 108.1 .
C4 C3 C2 120.8(3) .
C4 C3 H3 119.7 .
C2 C3 H3 119.5 .
C1 C6 C5 119.9(2) .
C1 C6 C10 119.8(2) .
C5 C6 C10 120.3(2) .
C3 C2 C1 119.7(2) .
C3 C2 C7 120.7(2) .
C1 C2 C7 119.7(2) .
N1 C8 H8A 109.6 .
N1 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
N1 C8 H8C 109.4 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C23 C24 C19 121.6(3) .
C23 C24 H24 119.3 .
C19 C24 H24 119.1 .
C24 C23 C22 120.0(3) .
C24 C23 H23 119.8 .
C22 C23 H23 120.3 .
C22 C21 C20 120.1(3) .
C22 C21 H21 120.0 .
C20 C21 H21 119.8 .
C21 C20 C19 121.7(3) .
C21 C20 H20 119.1 .
C19 C20 H20 119.2 .
C21 C22 C23 119.6(3) .
C21 C22 H22 120.3 .
C23 C22 H22 120.1 .
C16 C15 C14 120.1(3) .
C16 C15 H15 119.9 .
C14 C15 H15 119.9 .
C20 C19 C24 117.0(2) .
C20 C19 Si1 124.6(2) .
C24 C19 Si1 118.03(19) .
N2 C10 C6 110.6(2) .
N2 C10 H10A 109.4 .
C6 C10 H10A 109.6 .
N2 C10 H10B 109.5 .
C6 C10 H10B 109.5 .
H10A C10 H10B 108.1 .
C17 C18 C13 122.1(3) .
C17 C18 H18 119.0 .
C13 C18 H18 118.9 .
C15 C16 C17 120.0(3) .
C15 C16 H16 119.8 .
C17 C16 H16 120.2 .
N2 C12 H12A 109.6 .
N2 C12 H12B 109.5 .
H12A C12 H12B 109.5 .
N2 C12 H12C 109.4 .
H12A C12 H12C 109.5 .
H12B C12 H12C 109.5 .
C18 C17 C16 119.8(3) .
C18 C17 H17 120.1 .
C16 C17 H17 120.1 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 O2 1.9831(18) .
Sb1 O1 2.0063(17) .
Sb1 C1 2.167(2) .
Si1 O2 1.6055(19) 3_556
Si1 O1 1.6184(18) .
Si1 C19 1.876(3) .
Si1 C13 1.878(3) .
C13 C18 1.399(4) .
C13 C14 1.405(4) .
O2 Si1 1.6055(19) 3_556
N2 C12 1.454(4) .
N2 C11 1.458(4) .
N2 C10 1.464(3) .
C1 C6 1.393(4) .
C1 C2 1.404(4) .
N1 C9 1.458(4) .
N1 C7 1.465(3) .
N1 C8 1.465(3) .
C14 C15 1.390(4) .
C14 H14 0.9301 .
C4 C5 1.380(4) .
C4 C3 1.382(4) .
C4 H4 0.9300 .
C5 C6 1.398(4) .
C5 H5 0.9301 .
C9 H9A 0.9599 .
C9 H9B 0.9599 .
C9 H9C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9601 .
C11 H11C 0.9600 .
C7 C2 1.501(4) .
C7 H7A 0.9699 .
C7 H7B 0.9700 .
C3 C2 1.389(4) .
C3 H3 0.9301 .
C6 C10 1.507(4) .
C8 H8A 0.9601 .
C8 H8B 0.9599 .
C8 H8C 0.9600 .
C24 C23 1.380(4) .
C24 C19 1.398(4) .
C24 H24 0.9300 .
C23 C22 1.392(4) .
C23 H23 0.9300 .
C21 C22 1.370(4) .
C21 C20 1.385(4) .
C21 H21 0.9300 .
C20 C19 1.396(4) .
C20 H20 0.9301 .
C22 H22 0.9300 .
C15 C16 1.373(5) .
C15 H15 0.9300 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C18 C17 1.378(4) .
C18 H18 0.9300 .
C16 C17 1.383(5) .
C16 H16 0.9299 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C17 H17 0.9300 .
