#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:33:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179485 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/82/4338220.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_4338220
loop_
_publ_author_name
'König, Sonja N'
'Schädle, Christoph'
'Maichle-Mössmer, Cäcilia'
'Anwander, Reiner'
_publ_section_title
;
 Silylamide Complexes of Chromium(II), Manganese(II), and Cobalt(II)
 Bearing the Ligands N(SiHMe2)2 and N(SiPhMe2)2.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4585
_journal_page_last               4597
_journal_paper_doi               10.1021/ic5002682
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C16 H48 Co N4 Si4'
_chemical_formula_weight         467.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 104.1980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3416(3)
_cell_length_b                   14.7835(4)
_cell_length_c                   10.2637(3)
_cell_measurement_reflns_used    184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.41
_cell_measurement_theta_min      5.47
_cell_volume                     1374.14(7)
_computing_cell_refinement       SAINT
_computing_data_collection       COSMO
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'APEX II'
_diffrn_measurement_method       omega/phi
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28920
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  0.6830
_exptl_absorpt_correction_T_min  0.5505
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.059(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         8206
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0273P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                7968
_reflns_number_total             8206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5002682_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4338216--4338226.cif.'
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4338220
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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
Co1 Co 0.216946(12) 0.247861(8) 0.353569(11) 0.01532(3) Uani 1 1 d .
Si1 Si 0.48178(3) 0.232804(17) 0.62010(3) 0.02008(6) Uani 1 1 d .
Si2 Si 0.22113(3) 0.347993(18) 0.62300(3) 0.01867(5) Uani 1 1 d .
H1 H 0.5132(15) 0.1583(10) 0.5481(13) 0.032(4) Uiso 1 1 d .
H2 H 0.1202(17) 0.3938(11) 0.5349(15) 0.040(4) Uiso 1 1 d .
Si3 Si 0.21553(3) 0.441947(17) 0.22696(3) 0.01881(5) Uani 1 1 d .
Si4 Si -0.07229(3) 0.34405(2) 0.17436(3) 0.02984(7) Uani 1 1 d .
N1 N 0.31561(9) 0.27825(5) 0.54153(8) 0.01733(15) Uani 1 1 d .
N2 N 0.11420(9) 0.34678(6) 0.23816(8) 0.01982(16) Uani 1 1 d .
N4 N 0.32996(10) 0.17028(6) 0.22762(9) 0.02395(18) Uani 1 1 d .
N3 N 0.11653(10) 0.11548(6) 0.37641(9) 0.02245(17) Uani 1 1 d .
C1 C 0.64529(12) 0.30990(8) 0.63711(13) 0.0311(2) Uani 1 1 d .
H1A H 0.6478 0.3334 0.5484 0.047 Uiso 1 1 calc R
H1B H 0.7362 0.2761 0.6750 0.047 Uiso 1 1 calc R
H1C H 0.6371 0.3604 0.6967 0.047 Uiso 1 1 calc R
C2 C 0.48773(13) 0.18696(8) 0.79236(11) 0.0291(2) Uani 1 1 d .
H2A H 0.4703 0.2362 0.8505 0.044 Uiso 1 1 calc R
H2B H 0.5849 0.1601 0.8306 0.044 Uiso 1 1 calc R
H2C H 0.4111 0.1407 0.7857 0.044 Uiso 1 1 calc R
C3 C 0.11162(13) 0.28812(9) 0.72815(12) 0.0301(2) Uani 1 1 d .
H3A H 0.0382 0.2487 0.6706 0.045 Uiso 1 1 calc R
H3B H 0.0613 0.3328 0.7717 0.045 Uiso 1 1 calc R
H3C H 0.1782 0.2517 0.7969 0.045 Uiso 1 1 calc R
C4 C 0.34388(13) 0.43306(8) 0.73265(12) 0.0299(2) Uani 1 1 d .
H4A H 0.4207 0.4014 0.7992 0.045 Uiso 1 1 calc R
H4B H 0.2849 0.4703 0.7789 0.045 Uiso 1 1 calc R
H4C H 0.3900 0.4718 0.6770 0.045 Uiso 1 1 calc R
C5 C 0.14842(16) 0.54711(8) 0.29568(15) 0.0375(3) Uani 1 1 d .
H5A H 0.0519 0.5643 0.2387 0.056 Uiso 1 1 calc R
H5B H 0.2191 0.5963 0.2969 0.056 Uiso 1 1 calc R
H5C H 0.1392 0.5356 0.3873 0.056 Uiso 1 1 calc R
C6 C 0.41300(13) 0.43203(8) 0.32373(15) 0.0371(3) Uani 1 1 d .
H6A H 0.4171 0.4211 0.4187 0.056 Uiso 1 1 calc R
H6B H 0.4654 0.4883 0.3149 0.056 Uiso 1 1 calc R
H6C H 0.4598 0.3815 0.2881 0.056 Uiso 1 1 calc R
C7 C 0.22252(19) 0.46853(10) 0.04968(12) 0.0442(3) Uani 1 1 d .
H7A H 0.2733 0.4195 0.0149 0.066 Uiso 1 1 calc R
H7B H 0.2761 0.5254 0.0482 0.066 Uiso 1 1 calc R
H7C H 0.1218 0.4746 -0.0066 0.066 Uiso 1 1 calc R
C8 C -0.15381(19) 0.44684(13) 0.0747(3) 0.0846(8) Uani 1 1 d .
H8A H -0.1366 0.5002 0.1330 0.127 Uiso 1 1 calc R
H8B H -0.2602 0.4381 0.0391 0.127 Uiso 1 1 calc R
H8C H -0.1069 0.4557 0.0000 0.127 Uiso 1 1 calc R
C9 C -0.17563(14) 0.33574(10) 0.30864(16) 0.0442(3) Uani 1 1 d .
H9A H -0.1299 0.2895 0.3741 0.066 Uiso 1 1 calc R
H9B H -0.2785 0.3191 0.2681 0.066 Uiso 1 1 calc R
H9C H -0.1727 0.3943 0.3541 0.066 Uiso 1 1 calc R
C10 C -0.13369(14) 0.24967(12) 0.04926(12) 0.0432(3) Uani 1 1 d .
H10A H -0.0983 0.2616 -0.0315 0.065 Uiso 1 1 calc R
H10B H -0.2418 0.2463 0.0249 0.065 Uiso 1 1 calc R
H10C H -0.0929 0.1922 0.0894 0.065 Uiso 1 1 calc R
C11 C 0.30632(13) 0.07394(7) 0.25716(12) 0.0269(2) Uani 1 1 d .
H11A H 0.3768 0.0563 0.3421 0.032 Uiso 1 1 calc R
H11B H 0.3255 0.0355 0.1843 0.032 Uiso 1 1 calc R
C12 C 0.15021(13) 0.05831(7) 0.26949(12) 0.0273(2) Uani 1 1 d .
H12A H 0.0800 0.0724 0.1827 0.033 Uiso 1 1 calc R
H12B H 0.1377 -0.0062 0.2903 0.033 Uiso 1 1 calc R
C13 C 0.49022(14) 0.18564(9) 0.24535(13) 0.0335(3) Uani 1 1 d .
H13A H 0.5415 0.1759 0.3397 0.050 Uiso 1 1 calc R
H13B H 0.5069 0.2479 0.2196 0.050 Uiso 1 1 calc R
H13C H 0.5284 0.1433 0.1885 0.050 Uiso 1 1 calc R
C14 C 0.25748(15) 0.18981(8) 0.08391(11) 0.0320(2) Uani 1 1 d .
H14A H 0.2740 0.2533 0.0641 0.048 Uiso 1 1 calc R
H14B H 0.1512 0.1784 0.0673 0.048 Uiso 1 1 calc R
H14C H 0.2996 0.1506 0.0259 0.048 Uiso 1 1 calc R
C15 C 0.18755(14) 0.07611(7) 0.50981(12) 0.0304(2) Uani 1 1 d .
H15A H 0.1479 0.0154 0.5166 0.046 Uiso 1 1 calc R
H15B H 0.1671 0.1146 0.5808 0.046 Uiso 1 1 calc R
H15C H 0.2945 0.0724 0.5200 0.046 Uiso 1 1 calc R
C16 C -0.04388(13) 0.11406(8) 0.36618(13) 0.0314(2) Uani 1 1 d .
H16A H -0.0965 0.1392 0.2793 0.047 Uiso 1 1 calc R
H16B H -0.0655 0.1504 0.4389 0.047 Uiso 1 1 calc R
H16C H -0.0761 0.0516 0.3736 0.047 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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
N1 Co1 N2 117.32(3)
N1 Co1 N4 121.33(3)
N2 Co1 N4 105.55(4)
N1 Co1 N3 101.92(3)
N2 Co1 N3 124.27(3)
N4 Co1 N3 82.93(3)
N1 Si1 C1 115.51(5)
N1 Si1 C2 113.63(5)
C1 Si1 C2 107.17(5)
N1 Si1 H1 110.2(6)
C1 Si1 H1 104.8(6)
C2 Si1 H1 104.6(6)
N1 Si2 C4 112.67(5)
N1 Si2 C3 114.65(5)
C4 Si2 C3 108.02(5)
N1 Si2 H2 110.0(7)
C4 Si2 H2 107.1(7)
C3 Si2 H2 103.7(7)
N2 Si3 C6 112.83(5)
N2 Si3 C5 114.42(5)
C6 Si3 C5 103.99(6)
N2 Si3 C7 112.79(5)
C6 Si3 C7 105.44(7)
C5 Si3 C7 106.55(7)
N2 Si4 C9 112.46(5)
N2 Si4 C8 115.35(6)
C9 Si4 C8 103.89(10)
N2 Si4 C10 112.97(6)
C9 Si4 C10 109.09(6)
C8 Si4 C10 102.22(9)
Si1 N1 Si2 121.89(5)
Si1 N1 Co1 121.73(5)
Si2 N1 Co1 116.31(4)
Si4 N2 Si3 121.50(5)
Si4 N2 Co1 120.87(5)
Si3 N2 Co1 116.89(4)
C13 N4 C11 108.59(9)
C13 N4 C14 106.96(10)
C11 N4 C14 109.48(8)
C13 N4 Co1 117.89(7)
C11 N4 Co1 105.39(7)
C14 N4 Co1 108.38(7)
C16 N3 C12 109.64(9)
C16 N3 C15 106.02(9)
C12 N3 C15 109.38(9)
C16 N3 Co1 117.08(7)
C12 N3 Co1 104.75(6)
C15 N3 Co1 109.87(6)
Si1 C1 H1A 109.5
Si1 C1 H1B 109.5
H1A C1 H1B 109.5
Si1 C1 H1C 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
Si1 C2 H2A 109.5
Si1 C2 H2B 109.5
H2A C2 H2B 109.5
Si1 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
Si2 C3 H3A 109.5
Si2 C3 H3B 109.5
H3A C3 H3B 109.5
Si2 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
Si2 C4 H4A 109.5
Si2 C4 H4B 109.5
H4A C4 H4B 109.5
Si2 C4 H4C 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
Si3 C5 H5A 109.5
Si3 C5 H5B 109.5
H5A C5 H5B 109.5
Si3 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
Si3 C6 H6A 109.5
Si3 C6 H6B 109.5
H6A C6 H6B 109.5
Si3 C6 H6C 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
Si3 C7 H7A 109.5
Si3 C7 H7B 109.5
H7A C7 H7B 109.5
Si3 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
Si4 C8 H8A 109.5
Si4 C8 H8B 109.5
H8A C8 H8B 109.5
Si4 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
Si4 C9 H9A 109.5
Si4 C9 H9B 109.5
H9A C9 H9B 109.5
Si4 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
Si4 C10 H10A 109.5
Si4 C10 H10B 109.5
H10A C10 H10B 109.5
Si4 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
N4 C11 C12 111.02(9)
N4 C11 H11A 109.4
C12 C11 H11A 109.4
N4 C11 H11B 109.4
C12 C11 H11B 109.4
H11A C11 H11B 108.0
N3 C12 C11 111.09(9)
N3 C12 H12A 109.4
C11 C12 H12A 109.4
N3 C12 H12B 109.4
C11 C12 H12B 109.4
H12A C12 H12B 108.0
N4 C13 H13A 109.5
N4 C13 H13B 109.5
H13A C13 H13B 109.5
N4 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
N4 C14 H14A 109.5
N4 C14 H14B 109.5
H14A C14 H14B 109.5
N4 C14 H14C 109.5
H14A C14 H14C 109.5
H14B C14 H14C 109.5
N3 C15 H15A 109.5
N3 C15 H15B 109.5
H15A C15 H15B 109.5
N3 C15 H15C 109.5
H15A C15 H15C 109.5
H15B C15 H15C 109.5
N3 C16 H16A 109.5
N3 C16 H16B 109.5
H16A C16 H16B 109.5
N3 C16 H16C 109.5
H16A C16 H16C 109.5
H16B C16 H16C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 N1 1.9750(8)
Co1 N2 1.9761(8)
Co1 N4 2.1842(9)
Co1 N3 2.2075(8)
Co1 Si1 3.2146(3)
Co1 Si2 3.1284(3)
Co1 Si3 3.1485(3)
Co1 Si4 3.2043(3)
Si1 N1 1.7021(8)
Si1 C1 1.8794(12)
Si1 C2 1.8815(11)
Si1 H1 1.397(14)
Si2 N1 1.7040(8)
Si2 C4 1.8788(11)
Si2 C3 1.8804(11)
Si2 H2 1.322(15)
Si3 N2 1.7153(9)
Si3 C6 1.8740(13)
Si3 C5 1.8774(12)
Si3 C7 1.8782(12)
Si4 N2 1.7046(9)
Si4 C9 1.8706(15)
Si4 C8 1.8852(15)
Si4 C10 1.8876(15)
N4 C13 1.4806(15)
N4 C11 1.4839(14)
N4 C14 1.4925(15)
N3 C16 1.4765(15)
N3 C12 1.4787(14)
N3 C15 1.4859(14)
C1 H1A 0.9800
C1 H1B 0.9800
C1 H1C 0.9800
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
C3 H3A 0.9800
C3 H3B 0.9800
C3 H3C 0.9800
C4 H4A 0.9800
C4 H4B 0.9800
C4 H4C 0.9800
C5 H5A 0.9800
C5 H5B 0.9800
C5 H5C 0.9800
C6 H6A 0.9800
C6 H6B 0.9800
C6 H6C 0.9800
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 H9A 0.9800
C9 H9B 0.9800
C9 H9C 0.9800
C10 H10A 0.9800
C10 H10B 0.9800
C10 H10C 0.9800
C11 C12 1.5122(17)
C11 H11A 0.9900
C11 H11B 0.9900
C12 H12A 0.9900
C12 H12B 0.9900
C13 H13A 0.9800
C13 H13B 0.9800
C13 H13C 0.9800
C14 H14A 0.9800
C14 H14B 0.9800
C14 H14C 0.9800
C15 H15A 0.9800
C15 H15B 0.9800
C15 H15C 0.9800
C16 H16A 0.9800
C16 H16B 0.9800
C16 H16C 0.9800
