#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:23:13 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180180 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/76/7107627.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_7107627
loop_
_publ_author_name
'Ramachandran Azhakar'
'Rajendra S. Ghadwal'
'Herbert W. Roesky'
'Hilke Wolf'
'Dietmar Stalke'
_publ_section_title
;
 A d?but for base stabilized monoalkylsilylenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              4561
_journal_paper_doi               10.1039/c2cc31041d
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C38 H64 N4 O2 Si2'
_chemical_formula_sum            'C38 H64 N4 O2 Si2'
_chemical_formula_weight         665.11
_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                110.480(10)
_cell_angle_beta                 94.95(2)
_cell_angle_gamma                116.21(2)
_cell_formula_units_Z            1
_cell_length_a                   9.878(3)
_cell_length_b                   10.371(4)
_cell_length_c                   11.472(5)
_cell_measurement_reflns_used    9313
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.329
_cell_measurement_theta_min      2.376
_cell_volume                     946.4(7)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXS in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27594
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_correction_T_min  0.9374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0474P)²+0.3544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                4455
_reflns_number_total             4682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31041d.txt
_cod_data_source_block           sad_a
_cod_original_cell_volume        946.3(6)
_cod_database_code               7107627
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
Si1 Si 0.50991(3) 0.53454(3) 0.61758(2) 0.01302(8) Uani 1 1 d .
O1 O 0.44591(8) 0.57935(8) 0.50550(6) 0.01466(14) Uani 1 1 d .
N1 N 0.37275(9) 0.38149(10) 0.66067(8) 0.01368(16) Uani 1 1 d .
C1 C 0.30316(11) 0.46507(11) 0.71916(9) 0.01340(18) Uani 1 1 d .
N2 N 0.37932(9) 0.60774(10) 0.72466(8) 0.01417(16) Uani 1 1 d .
C2 C 0.15428(11) 0.39352(11) 0.75442(9) 0.01507(18) Uani 1 1 d .
C3 C 0.15343(12) 0.41187(12) 0.88050(10) 0.0193(2) Uani 1 1 d .
H3 H 0.2498 0.4738 0.9480 0.023 Uiso 1 1 calc R
C4 C 0.01162(14) 0.33951(14) 0.90757(12) 0.0258(2) Uani 1 1 d .
H4 H 0.0112 0.3500 0.9932 0.031 Uiso 1 1 calc R
C5 C -0.12949(14) 0.25184(14) 0.80951(13) 0.0287(3) Uani 1 1 d .
H5 H -0.2264 0.2036 0.8285 0.034 Uiso 1 1 calc R
C6 C -0.12942(13) 0.23444(13) 0.68423(12) 0.0255(2) Uani 1 1 d .
H6 H -0.2262 0.1751 0.6176 0.031 Uiso 1 1 calc R
C7 C 0.01186(12) 0.30357(12) 0.65593(10) 0.0194(2) Uani 1 1 d .
H7 H 0.0119 0.2898 0.5696 0.023 Uiso 1 1 calc R
C8 C 0.32704(12) 0.72637(12) 0.74867(10) 0.01654(19) Uani 1 1 d .
C9 C 0.29270(14) 0.77186(13) 0.88039(11) 0.0236(2) Uani 1 1 d .
H9A H 0.2768 0.8631 0.8998 0.035 Uiso 1 1 calc R
H9B H 0.3819 0.8004 0.9483 0.035 Uiso 1 1 calc R
H9C H 0.1975 0.6811 0.8773 0.035 Uiso 1 1 calc R
C10 C 0.18302(13) 0.66487(14) 0.63832(11) 0.0237(2) Uani 1 1 d .
H10A H 0.2071 0.6357 0.5551 0.035 Uiso 1 1 calc R
H10B H 0.1565 0.7487 0.6521 0.035 Uiso 1 1 calc R
H10C H 0.0934 0.5710 0.6373 0.035 Uiso 1 1 calc R
C11 C 0.46182(13) 0.87548(13) 0.74946(11) 0.0230(2) Uani 1 1 d .
H11A H 0.4888 0.8470 0.6675 0.035 Uiso 1 1 calc R
H11B H 0.5539 0.9207 0.8221 0.035 Uiso 1 1 calc R
H11C H 0.4291 0.9543 0.7593 0.035 Uiso 1 1 calc R
C12 C 0.36525(11) 0.24248(11) 0.67818(9) 0.01526(18) Uani 1 1 d .
C13 C 0.44503(14) 0.29613(13) 0.82078(10) 0.0227(2) Uani 1 1 d .
H13A H 0.4388 0.2045 0.8323 0.034 Uiso 1 1 calc R
H13B H 0.3914 0.3396 0.8765 0.034 Uiso 1 1 calc R
H13C H 0.5558 0.3784 0.8445 0.034 Uiso 1 1 calc R
C14 C 0.19608(12) 0.10371(12) 0.63672(11) 0.0216(2) Uani 1 1 d .
H14A H 0.1411 0.0800 0.5501 0.032 Uiso 1 1 calc R
H14B H 0.1410 0.1331 0.6990 0.032 Uiso 1 1 calc R
H14C H 0.1980 0.0092 0.6345 0.032 Uiso 1 1 calc R
C15 C 0.45335(12) 0.17983(12) 0.59284(10) 0.01847(19) Uani 1 1 d .
H15A H 0.4000 0.1400 0.5013 0.028 Uiso 1 1 calc R
H15B H 0.4549 0.0930 0.6078 0.028 Uiso 1 1 calc R
H15C H 0.5616 0.2663 0.6148 0.028 Uiso 1 1 calc R
C16 C 0.71358(11) 0.67888(12) 0.74291(9) 0.01668(19) Uani 1 1 d .
C17 C 0.71141(13) 0.75040(14) 0.88450(10) 0.0232(2) Uani 1 1 d .
H17A H 0.6619 0.8157 0.8934 0.035 Uiso 1 1 calc R
H17B H 0.8196 0.8170 0.9418 0.035 Uiso 1 1 calc R
H17C H 0.6513 0.6641 0.9085 0.035 Uiso 1 1 calc R
C18 C 0.81035(13) 0.59548(14) 0.73902(11) 0.0240(2) Uani 1 1 d .
H18A H 0.8136 0.5469 0.6499 0.036 Uiso 1 1 calc R
H18B H 0.7612 0.5125 0.7689 0.036 Uiso 1 1 calc R
H18C H 0.9178 0.6740 0.7958 0.036 Uiso 1 1 calc R
C19 C 0.80415(13) 0.81697(14) 0.70534(11) 0.0257(2) Uani 1 1 d .
H19A H 0.8109 0.7731 0.6167 0.039 Uiso 1 1 calc R
H19B H 0.9105 0.8892 0.7656 0.039 Uiso 1 1 calc R
H19C H 0.7483 0.8759 0.7100 0.039 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'
O O 0.0106 0.0060 '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'
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 85.21(5) . 2_666
O1 Si1 N1 121.37(5) . .
O1 Si1 N1 100.54(5) 2_666 .
O1 Si1 C16 121.44(5) . .
O1 Si1 C16 101.05(5) 2_666 .
N1 Si1 C16 114.54(5) . .
O1 Si1 N2 87.82(4) . .
O1 Si1 N2 159.96(4) 2_666 .
N1 Si1 N2 67.42(4) . .
C16 Si1 N2 98.62(5) . .
O1 Si1 C1 104.43(4) . .
O1 Si1 C1 132.25(4) 2_666 .
N1 Si1 C1 34.61(3) . .
C16 Si1 C1 111.91(5) . .
N2 Si1 C1 32.95(4) . .
O1 Si1 Si1 43.37(3) . 2_666
O1 Si1 Si1 41.84(3) 2_666 2_666
N1 Si1 Si1 118.33(4) . 2_666
C16 Si1 Si1 118.76(4) . 2_666
N2 Si1 Si1 128.46(3) . 2_666
C1 Si1 Si1 129.06(4) . 2_666
Si1 O1 Si1 94.79(5) . 2_666
C1 N1 C12 125.20(8) . .
C1 N1 Si1 95.82(7) . .
C12 N1 Si1 135.65(7) . .
N2 C1 N1 108.36(8) . .
N2 C1 C2 127.41(9) . .
N1 C1 C2 123.86(9) . .
N2 C1 Si1 59.09(5) . .
N1 C1 Si1 49.57(5) . .
C2 C1 Si1 167.82(7) . .
C1 N2 C8 128.01(9) . .
C1 N2 Si1 87.96(6) . .
C8 N2 Si1 138.71(6) . .
C3 C2 C7 119.65(10) . .
C3 C2 C1 122.28(9) . .
C7 C2 C1 118.07(9) . .
C4 C3 C2 119.98(10) . .
C5 C4 C3 120.02(11) . .
C6 C5 C4 120.22(10) . .
C5 C6 C7 120.07(11) . .
C6 C7 C2 120.03(10) . .
N2 C8 C11 106.98(8) . .
N2 C8 C9 111.73(8) . .
C11 C8 C9 108.58(9) . .
N2 C8 C10 110.88(8) . .
C11 C8 C10 107.67(9) . .
C9 C8 C10 110.80(9) . .
N1 C12 C15 108.85(8) . .
N1 C12 C14 112.56(8) . .
C15 C12 C14 107.03(9) . .
N1 C12 C13 109.61(8) . .
C15 C12 C13 108.84(8) . .
C14 C12 C13 109.85(9) . .
C17 C16 C18 106.84(9) . .
C17 C16 C19 108.70(9) . .
C18 C16 C19 106.94(9) . .
C17 C16 Si1 115.13(7) . .
C18 C16 Si1 110.74(7) . .
C19 C16 Si1 108.18(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O1 1.6752(9) .
Si1 O1 1.7245(9) 2_666
Si1 N1 1.8342(10) .
Si1 C16 1.9209(13) .
Si1 N2 2.0579(10) .
Si1 C1 2.3971(12) .
Si1 Si1 2.5025(13) 2_666
O1 Si1 1.7245(9) 2_666
N1 C1 1.3686(12) .
N1 C12 1.4950(13) .
C1 N2 1.3047(14) .
C1 C2 1.4920(13) .
N2 C8 1.4850(13) .
C2 C3 1.3925(15) .
C2 C7 1.3981(15) .
C3 C4 1.3898(15) .
C4 C5 1.3890(19) .
C5 C6 1.3846(19) .
C6 C7 1.3872(15) .
C8 C11 1.5275(15) .
C8 C9 1.5336(15) .
C8 C10 1.5349(16) .
C12 C15 1.5295(14) .
C12 C14 1.5328(15) .
C12 C13 1.5362(16) .
C16 C17 1.5381(15) .
C16 C18 1.5410(15) .
C16 C19 1.5504(15) .
