#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/38/7033856.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_7033856
loop_
_publ_author_name
'Kämpfe, Alexander'
'Brendler, Erica'
'Kroke, Edwin'
'Wagler, Jörg'
_publ_section_title
;
 Tp*Cu(i)-CN-SiL2-NC-Cu(i)Tp* - a hexacoordinate Si-complex as connector
 for redox active metals via π-conjugated ligands.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4744
_journal_page_last               4750
_journal_paper_doi               10.1039/c4dt03903c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C32 H32 N4 O2 S2 Si'
_chemical_formula_sum            'C32 H32 N4 O2 S2 Si'
_chemical_formula_weight         596.83
_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
_audit_update_record
;
2014-04-28 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.342(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2839(4)
_cell_length_b                   20.7778(13)
_cell_length_c                   10.4718(7)
_cell_measurement_reflns_used    11198
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.79
_cell_volume                     1548.21(17)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP32 (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'omega 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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11770
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.8972
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XShape
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0340
_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)+(0.0375P)²+0.6044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                2495
_reflns_number_total             3026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03903c2.cif
_cod_data_source_block           ak236b01
_cod_depositor_comments
'Adding full bibliography for 7033856--7033861.cif.'
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7033856
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
S1 S 0.68228(6) 0.36374(2) 0.20344(4) 0.04094(14) Uani 1 1 d .
Si1 Si 0.5000 0.5000 0.5000 0.02708(15) Uani 1 2 d S
O1 O 0.28672(15) 0.50721(5) 0.38333(10) 0.0306(3) Uani 1 1 d .
N1 N 0.57022(18) 0.57633(7) 0.43057(12) 0.0295(3) Uani 1 1 d .
N2 N 0.60001(19) 0.45228(7) 0.38097(13) 0.0334(3) Uani 1 1 d .
C1 C 0.7012(2) 0.62247(8) 0.45577(16) 0.0333(4) Uani 1 1 d .
C2 C 0.6528(2) 0.67391(8) 0.36504(16) 0.0334(4) Uani 1 1 d .
C3 C 0.4853(2) 0.65833(8) 0.28083(15) 0.0309(3) Uani 1 1 d .
C4 C 0.4315(2) 0.59687(8) 0.32317(14) 0.0279(3) Uani 1 1 d .
C5 C 0.8711(3) 0.61937(10) 0.56445(19) 0.0486(5) Uani 1 1 d .
H5A H 0.8326 0.6108 0.6470 0.073 Uiso 1 1 calc R
H5B H 0.9383 0.6605 0.5706 0.073 Uiso 1 1 calc R
H5C H 0.9539 0.5848 0.5471 0.073 Uiso 1 1 calc R
C6 C 0.7693(3) 0.73365(9) 0.36275(19) 0.0428(4) Uani 1 1 d .
H6A H 0.8205 0.7478 0.4537 0.051 Uiso 1 1 calc R
H6B H 0.6877 0.7685 0.3177 0.051 Uiso 1 1 calc R
C7 C 0.9318(3) 0.72304(12) 0.2937(3) 0.0668(7) Uani 1 1 d .
H7A H 1.0163 0.6900 0.3403 0.100 Uiso 1 1 calc R
H7B H 1.0011 0.7634 0.2929 0.100 Uiso 1 1 calc R
H7C H 0.8820 0.7089 0.2037 0.100 Uiso 1 1 calc R
C8 C 0.3865(3) 0.69858(9) 0.16787(17) 0.0412(4) Uani 1 1 d .
H8A H 0.4224 0.7438 0.1840 0.062 Uiso 1 1 calc R
H8B H 0.2503 0.6942 0.1583 0.062 Uiso 1 1 calc R
H8C H 0.4224 0.6840 0.0876 0.062 Uiso 1 1 calc R
C9 C 0.2777(2) 0.55583(8) 0.30062(14) 0.0283(3) Uani 1 1 d .
C10 C 0.1043(2) 0.56077(8) 0.19993(15) 0.0281(3) Uani 1 1 d .
C11 C 0.1067(2) 0.58135(8) 0.07325(16) 0.0333(4) Uani 1 1 d .
H11 H 0.2226 0.5918 0.0506 0.040 Uiso 1 1 calc R
C12 C -0.0591(3) 0.58656(9) -0.01893(17) 0.0404(4) Uani 1 1 d .
H12 H -0.0570 0.6008 -0.1049 0.049 Uiso 1 1 calc R
C13 C -0.2289(3) 0.57113(9) 0.01349(18) 0.0431(4) Uani 1 1 d .
H13 H -0.3432 0.5758 -0.0495 0.052 Uiso 1 1 calc R
C14 C -0.2316(2) 0.54894(9) 0.13790(18) 0.0391(4) Uani 1 1 d .
H14 H -0.3477 0.5377 0.1594 0.047 Uiso 1 1 calc R
C15 C -0.0669(2) 0.54306(8) 0.23069(16) 0.0327(4) Uani 1 1 d .
H15 H -0.0694 0.5270 0.3153 0.039 Uiso 1 1 calc R
C16 C 0.6337(2) 0.41485(8) 0.30672(15) 0.0291(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
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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 '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
O1 Si1 O1 180.000(1) . 3_666
O1 Si1 N2 89.67(5) . .
O1 Si1 N2 90.33(6) 3_666 .
O1 Si1 N2 90.33(6) . 3_666
O1 Si1 N2 89.67(5) 3_666 3_666
N2 Si1 N2 180.0 . 3_666
O1 Si1 N1 93.90(5) . 3_666
O1 Si1 N1 86.10(5) 3_666 3_666
N2 Si1 N1 89.27(6) . 3_666
N2 Si1 N1 90.73(6) 3_666 3_666
O1 Si1 N1 86.10(5) . .
O1 Si1 N1 93.90(5) 3_666 .
N2 Si1 N1 90.73(6) . .
N2 Si1 N1 89.27(6) 3_666 .
N1 Si1 N1 180.00(4) 3_666 .
C9 O1 Si1 115.52(10) . .
C1 N1 C4 107.46(13) . .
C1 N1 Si1 141.00(11) . .
C4 N1 Si1 111.10(10) . .
C16 N2 Si1 167.02(13) . .
N1 C1 C2 110.00(14) . .
N1 C1 C5 123.99(15) . .
C2 C1 C5 126.01(15) . .
C3 C2 C1 107.99(14) . .
C3 C2 C6 127.31(15) . .
C1 C2 C6 124.69(15) . .
C2 C3 C4 105.89(14) . .
C2 C3 C8 125.55(15) . .
C4 C3 C8 128.55(15) . .
C9 C4 N1 111.41(13) . .
C9 C4 C3 139.41(15) . .
N1 C4 C3 108.65(13) . .
C1 C5 H5A 109.5 . .
C1 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C1 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C2 C6 C7 112.61(16) . .
C2 C6 H6A 109.1 . .
C7 C6 H6A 109.1 . .
C2 C6 H6B 109.1 . .
C7 C6 H6B 109.1 . .
H6A C6 H6B 107.8 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C3 C8 H8A 109.5 . .
C3 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C3 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O1 C9 C4 115.65(13) . .
O1 C9 C10 116.03(13) . .
C4 C9 C10 128.28(14) . .
C11 C10 C15 119.36(14) . .
C11 C10 C9 121.40(14) . .
C15 C10 C9 119.23(14) . .
C12 C11 C10 120.13(16) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C11 C12 C13 120.19(16) . .
C11 C12 H12 119.9 . .
C13 C12 H12 119.9 . .
C14 C13 C12 119.92(16) . .
C14 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C15 C14 C13 120.48(16) . .
C15 C14 H14 119.8 . .
C13 C14 H14 119.8 . .
C14 C15 C10 119.84(15) . .
C14 C15 H15 120.1 . .
C10 C15 H15 120.1 . .
N2 C16 S1 179.24(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C16 1.6081(17) .
Si1 O1 1.7655(10) .
Si1 O1 1.7655(10) 3_666
Si1 N2 1.8589(14) .
Si1 N2 1.8589(14) 3_666
Si1 N1 1.8613(13) 3_666
Si1 N1 1.8613(13) .
O1 C9 1.3232(19) .
N1 C1 1.338(2) .
N1 C4 1.4081(19) .
N2 C16 1.163(2) .
C1 C2 1.423(2) .
C1 C5 1.493(2) .
C2 C3 1.382(2) .
C2 C6 1.507(2) .
C3 C4 1.434(2) .
C3 C8 1.501(2) .
C4 C9 1.387(2) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C7 1.529(3) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.466(2) .
C10 C11 1.397(2) .
C10 C15 1.402(2) .
C11 C12 1.379(2) .
C11 H11 0.9500 .
C12 C13 1.389(3) .
C12 H12 0.9500 .
C13 C14 1.386(3) .
C13 H13 0.9500 .
C14 C15 1.378(2) .
C14 H14 0.9500 .
C15 H15 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N2 Si1 O1 C9 -86.34(11) .
N2 Si1 O1 C9 93.66(11) 3_666
N1 Si1 O1 C9 -175.59(11) 3_666
N1 Si1 O1 C9 4.41(11) .
O1 Si1 N1 C1 167.58(19) .
O1 Si1 N1 C1 -12.42(19) 3_666
N2 Si1 N1 C1 -102.80(19) .
N2 Si1 N1 C1 77.20(19) 3_666
O1 Si1 N1 C4 -3.38(10) .
O1 Si1 N1 C4 176.62(10) 3_666
N2 Si1 N1 C4 86.24(11) .
N2 Si1 N1 C4 -93.76(11) 3_666
O1 Si1 N2 C16 -57.7(6) .
O1 Si1 N2 C16 122.3(6) 3_666
N1 Si1 N2 C16 36.2(6) 3_666
N1 Si1 N2 C16 -143.8(6) .
C4 N1 C1 C2 -0.61(18) .
Si1 N1 C1 C2 -171.76(14) .
C4 N1 C1 C5 178.98(17) .
Si1 N1 C1 C5 7.8(3) .
N1 C1 C2 C3 -0.13(19) .
C5 C1 C2 C3 -179.70(17) .
N1 C1 C2 C6 -179.10(16) .
C5 C1 C2 C6 1.3(3) .
C1 C2 C3 C4 0.79(18) .
C6 C2 C3 C4 179.72(16) .
C1 C2 C3 C8 -178.33(16) .
C6 C2 C3 C8 0.6(3) .
C1 N1 C4 C9 -172.24(14) .
Si1 N1 C4 C9 1.81(16) .
C1 N1 C4 C3 1.11(17) .
Si1 N1 C4 C3 175.15(10) .
C2 C3 C4 C9 169.28(19) .
C8 C3 C4 C9 -11.6(3) .
C2 C3 C4 N1 -1.17(17) .
C8 C3 C4 N1 177.92(16) .
C3 C2 C6 C7 -97.7(2) .
C1 C2 C6 C7 81.1(2) .
Si1 O1 C9 C4 -4.48(17) .
Si1 O1 C9 C10 177.59(10) .
N1 C4 C9 O1 1.55(19) .
C3 C4 C9 O1 -168.73(18) .
N1 C4 C9 C10 179.18(14) .
C3 C4 C9 C10 8.9(3) .
O1 C9 C10 C11 -143.62(15) .
C4 C9 C10 C11 38.8(2) .
O1 C9 C10 C15 34.9(2) .
C4 C9 C10 C15 -142.72(17) .
C15 C10 C11 C12 2.6(2) .
C9 C10 C11 C12 -178.92(16) .
C10 C11 C12 C13 -0.3(3) .
C11 C12 C13 C14 -1.6(3) .
C12 C13 C14 C15 1.1(3) .
C13 C14 C15 C10 1.2(3) .
C11 C10 C15 C14 -3.0(2) .
C9 C10 C15 C14 178.44(15) .
