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#$Date: 2025-08-22 01:24:23 +0300 (Fri, 22 Aug 2025) $
#$Revision: 301857 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/41/7114182.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_7114182
loop_
_publ_author_name
'Mund, Garry'
'Gabert, Andrea J.'
'Batchelor, Raymond J.'
'Britten, James F.'
'Leznoff, Daniel B.'
_publ_section_title
;
 A rare ether-bridged cobalt complex which gives rise to an unusual
 ???serpentine??? metal???ligand binding motif
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2990
_journal_paper_doi               10.1039/b208221g
_journal_year                    2002
_chemical_formula_sum            'C44 H68 Co2 N4 O2 Si4'
_chemical_formula_weight         915.24
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 107.854(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.132(11)
_cell_length_b                   13.972(8)
_cell_length_c                   19.761(12)
_cell_measurement_reflns_used    850
_cell_measurement_temperature    153.0(2)
_cell_measurement_theta_max      19.01
_cell_measurement_theta_min      2.58
_cell_volume                     4765(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1680
_diffrn_reflns_av_sigmaI/netI    0.1582
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12941
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1760
_refine_ls_R_factor_gt           0.0986
_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)+(0.0667P)²+48.3242P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2095
_reflns_number_gt                1756
_reflns_number_total             3068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208221g.txt
_cod_data_source_block           lez04
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7114182
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Co1 Co 0.06016(7) 0.19016(9) 0.23319(8) 0.0320(6) Uani 1 1 d .
Si1 Si 0.1952(2) 0.3199(3) 0.3152(2) 0.0593(12) Uani 1 1 d .
Si2 Si 0.10609(16) 0.20886(19) 0.40270(18) 0.0357(9) Uani 1 1 d .
O1 O 0.1508(5) 0.2919(6) 0.3738(4) 0.060(3) Uani 1 1 d .
N1 N 0.1359(4) 0.2853(5) 0.2330(5) 0.0307(17) Uani 1 1 d .
N2 N 0.0451(4) 0.1474(5) 0.3273(5) 0.0307(17) Uani 1 1 d .
C10 C 0.1438(5) 0.3277(6) 0.1713(6) 0.030(3) Uani 1 1 d .
C11 C 0.1023(6) 0.4095(7) 0.1438(7) 0.041(3) Uani 1 1 d .
C12 C 0.1100(7) 0.4526(8) 0.0855(9) 0.063(4) Uani 1 1 d .
H12A H 0.0831 0.5110 0.0704 0.075 Uiso 1 1 calc R
C13 C 0.1560(8) 0.4153(9) 0.0455(8) 0.062(4) Uani 1 1 d .
C14 C 0.1971(6) 0.3323(8) 0.0746(7) 0.051(4) Uani 1 1 d .
H14A H 0.2312 0.3057 0.0514 0.061 Uiso 1 1 calc R
C15 C 0.1913(6) 0.2872(7) 0.1339(7) 0.037(3) Uani 1 1 d .
C16 C 0.2143(9) 0.4511(9) 0.3223(8) 0.093(6) Uani 1 1 d .
H16A H 0.1649 0.4858 0.3100 0.139 Uiso 1 1 calc R
H16B H 0.2429 0.4696 0.2896 0.139 Uiso 1 1 calc R
H16C H 0.2450 0.4670 0.3711 0.139 Uiso 1 1 calc R
C17 C 0.2922(7) 0.2562(11) 0.3399(9) 0.095(6) Uani 1 1 d .
H17A H 0.2837 0.1869 0.3370 0.143 Uiso 1 1 calc R
H17B H 0.3225 0.2736 0.3885 0.143 Uiso 1 1 calc R
H17C H 0.3203 0.2753 0.3069 0.143 Uiso 1 1 calc R
C20 C 0.0414(5) 0.0452(7) 0.3410(6) 0.033(3) Uani 1 1 d .
C21 C 0.0913(5) -0.0197(7) 0.3200(6) 0.031(3) Uani 1 1 d .
C22 C 0.0840(6) -0.1182(7) 0.3303(7) 0.045(3) Uani 1 1 d .
H22A H 0.1175 -0.1608 0.3163 0.054 Uiso 1 1 calc R
C23 C 0.0306(6) -0.1560(6) 0.3595(7) 0.041(3) Uani 1 1 d .
C24 C -0.0162(6) -0.0922(7) 0.3820(7) 0.044(3) Uani 1 1 d .
H24A H -0.0528 -0.1163 0.4033 0.053 Uiso 1 1 calc R
C25 C -0.0103(6) 0.0065(7) 0.3739(6) 0.036(3) Uani 1 1 d .
C26 C 0.0554(7) 0.2694(8) 0.4581(7) 0.061(4) Uani 1 1 d .
H26A H 0.0174 0.3145 0.4288 0.091 Uiso 1 1 calc R
H26B H 0.0930 0.3043 0.4965 0.091 Uiso 1 1 calc R
H26C H 0.0287 0.2218 0.4785 0.091 Uiso 1 1 calc R
C27 C 0.1765(6) 0.1256(8) 0.4611(7) 0.057(4) Uani 1 1 d .
H27A H 0.2046 0.0916 0.4332 0.085 Uiso 1 1 calc R
H27B H 0.1489 0.0793 0.4818 0.085 Uiso 1 1 calc R
H27C H 0.2133 0.1617 0.4993 0.085 Uiso 1 1 calc R
C111 C 0.0461(7) 0.4556(9) 0.1769(9) 0.080(5) Uani 1 1 d .
H11A H 0.0233 0.5126 0.1495 0.120 Uiso 1 1 calc R
H11B H 0.0737 0.4740 0.2260 0.120 Uiso 1 1 calc R
H11C H 0.0050 0.4100 0.1766 0.120 Uiso 1 1 calc R
C131 C 0.1608(9) 0.4600(11) -0.0235(8) 0.108(7) Uani 1 1 d .
H13A H 0.1955 0.4218 -0.0422 0.161 Uiso 1 1 calc R
H13B H 0.1809 0.5254 -0.0142 0.161 Uiso 1 1 calc R
H13C H 0.1091 0.4615 -0.0585 0.161 Uiso 1 1 calc R
C151 C 0.2378(6) 0.1988(8) 0.1603(8) 0.074(5) Uani 1 1 d .
H15A H 0.2668 0.1815 0.1276 0.111 Uiso 1 1 calc R
H15B H 0.2030 0.1463 0.1630 0.111 Uiso 1 1 calc R
H15C H 0.2742 0.2109 0.2077 0.111 Uiso 1 1 calc R
C211 C 0.1547(6) 0.0133(7) 0.2890(7) 0.044(3) Uani 1 1 d .
H21A H 0.1811 -0.0428 0.2776 0.066 Uiso 1 1 calc R
H21B H 0.1922 0.0530 0.3240 0.066 Uiso 1 1 calc R
H21C H 0.1314 0.0506 0.2458 0.066 Uiso 1 1 calc R
C231 C 0.0235(7) -0.2648(8) 0.3684(8) 0.070(5) Uani 1 1 d .
H23A H -0.0175 -0.2777 0.3900 0.104 Uiso 1 1 calc R
H23B H 0.0728 -0.2900 0.3992 0.104 Uiso 1 1 calc R
H23C H 0.0106 -0.2958 0.3218 0.104 Uiso 1 1 calc R
C251 C -0.0597(6) 0.0706(7) 0.4065(7) 0.047(3) Uani 1 1 d .
H25A H -0.0919 0.0304 0.4268 0.070 Uiso 1 1 calc R
H25B H -0.0931 0.1117 0.3694 0.070 Uiso 1 1 calc R
H25C H -0.0256 0.1105 0.4439 0.070 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Co1 N2 139.3(4) . 2
N1 Co1 N2 120.0(4) . .
N2 Co1 N2 95.0(4) 2 .
N1 Co1 Co1 134.0(2) . 2
N2 Co1 Co1 53.3(2) 2 2
N2 Co1 Co1 51.7(2) . 2
O1 Si1 N1 107.4(4) . .
O1 Si1 C16 107.5(6) . .
N1 Si1 C16 113.3(6) . .
O1 Si1 C17 108.8(6) . .
N1 Si1 C17 111.9(6) . .
C16 Si1 C17 107.8(7) . .
O1 Si2 N2 107.5(4) . .
O1 Si2 C26 106.1(5) . .
N2 Si2 C26 115.1(5) . .
O1 Si2 C27 110.4(5) . .
N2 Si2 C27 110.6(4) . .
C26 Si2 C27 107.1(6) . .
Si2 O1 Si1 145.6(6) . .
C10 N1 Si1 120.1(6) . .
C10 N1 Co1 124.1(6) . .
Si1 N1 Co1 115.8(5) . .
C20 N2 Si2 111.7(7) . .
C20 N2 Co1 108.2(6) . 2
Si2 N2 Co1 126.1(4) . 2
C20 N2 Co1 118.6(7) . .
Si2 N2 Co1 113.4(4) . .
Co1 N2 Co1 74.9(3) 2 .
C11 C10 N1 120.2(9) . .
C11 C10 C15 118.0(10) . .
N1 C10 C15 121.8(8) . .
C12 C11 C10 121.4(11) . .
C12 C11 C111 116.1(11) . .
C10 C11 C111 122.5(12) . .
C11 C12 C13 123.2(11) . .
C14 C13 C12 114.0(12) . .
C14 C13 C131 122.4(15) . .
C12 C13 C131 123.6(14) . .
C15 C14 C13 124.2(12) . .
C14 C15 C10 119.1(9) . .
C14 C15 C151 119.7(11) . .
C10 C15 C151 121.1(11) . .
C25 C20 C21 117.5(9) . .
C25 C20 N2 122.5(9) . .
C21 C20 N2 120.0(9) . .
C22 C21 C20 119.0(9) . .
C22 C21 C211 117.9(9) . .
C20 C21 C211 123.1(9) . .
C23 C22 C21 123.2(10) . .
C22 C23 C24 117.6(9) . .
C22 C23 C231 121.4(10) . .
C24 C23 C231 120.9(10) . .
C23 C24 C25 121.3(10) . .
C24 C25 C20 121.3(10) . .
C24 C25 C251 116.8(10) . .
C20 C25 C251 121.8(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 1.912(7) .
Co1 N2 2.007(8) 2
Co1 N2 2.050(9) .
Co1 Co1 2.468(3) 2
Si1 O1 1.645(8) .
Si1 N1 1.720(9) .
Si1 C16 1.863(11) .
Si1 C17 1.897(14) .
Si2 O1 1.617(7) .
Si2 N2 1.780(9) .
Si2 C26 1.838(11) .
Si2 C27 1.847(12) .
N1 C10 1.401(12) .
N2 C20 1.459(12) .
N2 Co1 2.007(8) 2
C10 C11 1.385(14) .
C10 C15 1.414(14) .
C11 C12 1.344(17) .
C11 C111 1.514(16) .
C12 C13 1.413(18) .
C13 C14 1.403(17) .
C13 C131 1.527(18) .
C14 C15 1.364(15) .
C15 C151 1.496(15) .
C20 C25 1.404(14) .
C20 C21 1.428(13) .
C21 C22 1.404(13) .
C21 C211 1.529(13) .
C22 C23 1.375(14) .
C23 C24 1.394(14) .
C23 C231 1.540(14) .
C24 C25 1.395(13) .
C25 C251 1.542(14) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139184922
