#------------------------------------------------------------------------------
#$Date: 2018-08-27 04:33:40 +0300 (Mon, 27 Aug 2018) $
#$Revision: 210179 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/09/4300961.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_4300961
loop_
_publ_author_name
'Sydora, Orson L.'
'Wolczanski, Peter T.'
'Lobkovsky, Emil B.'
'Buda, Corneliu'
'Cundari, Thomas R.'
_publ_section_title
;
 Low-Coordinate Chromium Siloxides: The "Box" [Cr(μ-Cl)(μ-OSitBu3)]4,
 Distorted Trigonal [(tBu3SiO)3Cr][Na(benzene)] and
 [(tBu3SiO)3Cr][Na(dibenzo-18-c-6)], and Trigonal (tBu3SiO)3Cr
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2606
_journal_page_last               2618
_journal_paper_doi               10.1021/ic0488334
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C24 H54 Cl2 Cr2 O2 Si2'
_chemical_formula_weight         605.75
_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                 107.21(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.333(18)
_cell_length_b                   13.574(16)
_cell_length_c                   22.32(2)
_cell_measurement_temperature    173(2)
_cell_volume                     6463(11)
_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      173(2)
_diffrn_measured_fraction_theta_full 1.017
_diffrn_measured_fraction_theta_max 1.026
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8203
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.277
_refine_diff_density_min         -2.571
_refine_diff_density_rms         0.635
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.450
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3478
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.475
_refine_ls_R_factor_all          0.1698
_refine_ls_R_factor_gt           0.1227
_refine_ls_shift/su_max          4.238
_refine_ls_shift/su_mean         0.561
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3516
_refine_ls_wR_factor_ref         0.3903
_reflns_number_gt                2180
_reflns_number_total             3478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0488334si20040823_044937.cif
_cod_data_source_block           test
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4300961
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.0000 0.57450(18) 0.2500 0.0505(8) Uani 1 2 d S . .
Cr2 Cr 0.0000 0.29503(18) 0.2500 0.0440(7) Uani 1 2 d S . .
Cr3 Cr -0.06821(8) 0.43384(13) 0.17568(9) 0.0474(6) Uani 1 1 d . . .
Cl2 Cl 0.00110(14) 0.5421(2) 0.14492(16) 0.0554(9) Uani 1 1 d . . .
Cl1 Cl -0.10695(13) 0.3281(2) 0.24054(14) 0.0495(8) Uani 1 1 d . . .
Si1 Si -0.03592(19) 0.2314(3) 0.09523(19) 0.0710(12) Uani 1 1 d D . .
Si2 Si -0.15823(19) 0.6283(3) 0.1933(2) 0.0992(15) Uani 1 1 d D . .
O1 O -0.0305(4) 0.3067(6) 0.1571(3) 0.049(2) Uani 1 1 d . . .
O2 O -0.0938(3) 0.5605(5) 0.2104(4) 0.060(2) Uani 1 1 d . . .
C24 C -0.2530(6) 0.6767(10) 0.2528(7) 0.118(7) Uani 1 1 d D . .
H24A H -0.2749 0.6551 0.2826 0.178 Uiso 1 1 calc R . .
H24B H -0.2833 0.6863 0.2114 0.178 Uiso 1 1 calc R . .
H24C H -0.2312 0.7389 0.2673 0.178 Uiso 1 1 calc R . .
C23 C -0.1696(6) 0.5586(12) 0.3113(6) 0.122(7) Uani 1 1 d D . .
H23A H -0.1983 0.5465 0.3363 0.183 Uiso 1 1 calc R . .
H23B H -0.1375 0.6061 0.3331 0.183 Uiso 1 1 calc R . .
H23C H -0.1495 0.4966 0.3056 0.183 Uiso 1 1 calc R . .
C8 C -0.0470(7) 0.0813(13) 0.1801(7) 0.277(11) Uani 1 1 d D . .
H8A H -0.0336 0.0165 0.1985 0.416 Uiso 1 1 calc R . .
H8B H -0.0923 0.0808 0.1598 0.416 Uiso 1 1 calc R . .
H8C H -0.0366 0.1315 0.2131 0.416 Uiso 1 1 calc R . .
C7 C -0.0223(11) 0.0203(11) 0.0834(8) 0.269(18) Uani 1 1 d D . .
H7A H -0.0067 -0.0411 0.1057 0.403 Uiso 1 1 calc R . .
H7B H 0.0007 0.0343 0.0532 0.403 Uiso 1 1 calc R . .
H7C H -0.0671 0.0135 0.0612 0.403 Uiso 1 1 calc R . .
C6 C 0.0594(6) 0.1048(16) 0.1678(11) 0.31(2) Uani 1 1 d D . .
H6A H 0.0718 0.0387 0.1846 0.472 Uiso 1 1 calc R . .
H6B H 0.0676 0.1522 0.2024 0.472 Uiso 1 1 calc R . .
H6C H 0.0836 0.1231 0.1393 0.472 Uiso 1 1 calc R . .
C5 C -0.0127(7) 0.1052(8) 0.1308(6) 0.28(2) Uani 1 1 d D . .
C21 C -0.2056(5) 0.5991(10) 0.2485(5) 0.157(9) Uani 1 1 d D . .
C19 C -0.0884(10) 0.7855(16) 0.2530(7) 0.58(4) Uani 1 1 d D . .
H19A H -0.0754 0.8546 0.2546 0.868 Uiso 1 1 calc R . .
H19B H -0.0517 0.7428 0.2586 0.868 Uiso 1 1 calc R . .
H19C H -0.1074 0.7727 0.2866 0.868 Uiso 1 1 calc R . .
C18 C -0.1027(7) 0.7727(13) 0.1380(7) 0.206(10) Uani 1 1 d D . .
H18A H -0.0909 0.8414 0.1343 0.309 Uiso 1 1 calc R . .
H18B H -0.1314 0.7507 0.0979 0.309 Uiso 1 1 calc R . .
H18C H -0.0651 0.7313 0.1489 0.309 Uiso 1 1 calc R . .
C4 C 0.0932(7) 0.3015(13) 0.1072(6) 0.144(8) Uani 1 1 d D . .
H4A H 0.1230 0.3247 0.0858 0.216 Uiso 1 1 calc R . .
H4B H 0.1093 0.2415 0.1308 0.216 Uiso 1 1 calc R . .
H4C H 0.0874 0.3526 0.1361 0.216 Uiso 1 1 calc R . .
C22 C -0.2458(11) 0.5093(13) 0.2100(13) 0.49(5) Uani 1 1 d D . .
H22A H -0.2742 0.4842 0.2326 0.734 Uiso 1 1 calc R . .
H22B H -0.2175 0.4566 0.2055 0.734 Uiso 1 1 calc R . .
H22C H -0.2704 0.5323 0.1684 0.734 Uiso 1 1 calc R . .
C1 C 0.0309(5) 0.2796(9) 0.0591(6) 0.132(8) Uani 1 1 d D . .
C3 C 0.0384(10) 0.1998(11) 0.0121(7) 0.212(10) Uani 1 1 d D . .
H3A H 0.0707 0.2206 -0.0069 0.317 Uiso 1 1 calc R . .
H3B H -0.0015 0.1911 -0.0208 0.317 Uiso 1 1 calc R . .
H3C H 0.0509 0.1374 0.0343 0.317 Uiso 1 1 calc R . .
C17 C -0.1357(6) 0.7642(8) 0.1901(7) 0.41(2) Uani 1 1 d D . .
C15 C -0.2093(10) 0.4777(9) 0.0933(12) 0.263(16) Uani 1 1 d D . .
H15A H -0.2342 0.4665 0.0496 0.395 Uiso 1 1 calc R . .
H15B H -0.2294 0.4449 0.1214 0.395 Uiso 1 1 calc R . .
H15C H -0.1671 0.4508 0.1001 0.395 Uiso 1 1 calc R . .
C14 C -0.2723(6) 0.6316(15) 0.0892(11) 0.242(14) Uani 1 1 d D . .
H14A H -0.2959 0.6106 0.0468 0.363 Uiso 1 1 calc R . .
H14B H -0.2697 0.7037 0.0908 0.363 Uiso 1 1 calc R . .
H14C H -0.2937 0.6083 0.1191 0.363 Uiso 1 1 calc R . .
C13 C -0.2050(7) 0.5874(11) 0.1067(5) 0.208(14) Uani 1 1 d D . .
C2 C 0.0084(10) 0.3740(11) 0.0200(10) 0.330(16) Uani 1 1 d D . .
H2A H 0.0414 0.3972 0.0026 0.496 Uiso 1 1 calc R . .
H2B H -0.0008 0.4252 0.0469 0.496 Uiso 1 1 calc R . .
H2C H -0.0295 0.3593 -0.0143 0.496 Uiso 1 1 calc R . .
C20 C -0.1895(7) 0.8380(12) 0.1742(11) 0.302(14) Uani 1 1 d D . .
H20A H -0.1728 0.9048 0.1741 0.452 Uiso 1 1 calc R . .
H20B H -0.2121 0.8338 0.2057 0.452 Uiso 1 1 calc R . .
H20C H -0.2183 0.8230 0.1327 0.452 Uiso 1 1 calc R . .
C16 C -0.1711(8) 0.6370(17) 0.0628(11) 0.34(2) Uani 1 1 d D . .
H16A H -0.1925 0.6190 0.0192 0.504 Uiso 1 1 calc R . .
H16B H -0.1275 0.6144 0.0741 0.504 Uiso 1 1 calc R . .
H16C H -0.1720 0.7087 0.0675 0.504 Uiso 1 1 calc R . .
C12 C -0.1360(11) 0.2000(14) -0.0280(8) 0.290(18) Uani 1 1 d D . .
H12A H -0.1754 0.2294 -0.0535 0.435 Uiso 1 1 calc R . .
H12B H -0.1430 0.1306 -0.0201 0.435 Uiso 1 1 calc R . .
H12C H -0.1044 0.2049 -0.0504 0.435 Uiso 1 1 calc R . .
C11 C -0.0851(10) 0.3557(15) 0.0138(11) 0.53(4) Uani 1 1 d D . .
H11C H -0.0479 0.3404 0.0007 0.632 Uiso 1 1 calc R . .
H11A H -0.0735 0.4010 0.0495 0.790 Uiso 1 1 calc R . .
H11B H -0.1169 0.3865 -0.0212 0.790 Uiso 1 1 calc R . .
C10 C -0.1653(8) 0.286(2) 0.0588(9) 0.43(3) Uani 1 1 d D . .
H10A H -0.2019 0.3036 0.0237 0.644 Uiso 1 1 calc R . .
H10C H -0.1519 0.3434 0.0862 0.644 Uiso 1 1 calc R . .
H10D H -0.1762 0.2320 0.0827 0.644 Uiso 1 1 calc R . .
C9 C -0.1131(6) 0.2545(14) 0.0341(8) 0.57(4) Uani 1 1 d 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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
_geom_angle_publ_flag
O2 Cr1 O2 169.2(4) . 2 ?
O2 Cr1 Cl2 82.2(3) . . ?
O2 Cr1 Cl2 95.8(3) 2 . ?
O2 Cr1 Cl2 95.8(3) . 2 ?
O2 Cr1 Cl2 82.2(3) 2 2 ?
Cl2 Cr1 Cl2 158.81(18) . 2 ?
O2 Cr1 Cr3 48.7(2) . . ?
O2 Cr1 Cr3 121.8(2) 2 . ?
Cl2 Cr1 Cr3 55.45(9) . . ?
Cl2 Cr1 Cr3 107.81(12) 2 . ?
O2 Cr1 Cr3 121.8(2) . 2 ?
O2 Cr1 Cr3 48.7(2) 2 2 ?
Cl2 Cr1 Cr3 107.81(12) . 2 ?
Cl2 Cr1 Cr3 55.45(9) 2 2 ?
Cr3 Cr1 Cr3 89.46(13) . 2 ?
O1 Cr2 O1 170.8(5) . 2 ?
O1 Cr2 Cl1 82.4(2) . . ?
O1 Cr2 Cl1 95.9(2) 2 . ?
O1 Cr2 Cl1 95.9(2) . 2 ?
O1 Cr2 Cl1 82.4(2) 2 2 ?
Cl1 Cr2 Cl1 158.23(18) . 2 ?
O1 Cr2 Cr3 48.6(2) . . ?
O1 Cr2 Cr3 123.2(2) 2 . ?
Cl1 Cr2 Cr3 55.80(9) . . ?
Cl1 Cr2 Cr3 107.19(12) 2 . ?
O1 Cr2 Cr3 123.2(2) . 2 ?
O1 Cr2 Cr3 48.6(2) 2 2 ?
Cl1 Cr2 Cr3 107.19(12) . 2 ?
Cl1 Cr2 Cr3 55.80(9) 2 2 ?
Cr3 Cr2 Cr3 90.22(14) . 2 ?
O1 Cr3 O2 169.2(3) . . ?
O1 Cr3 Cl1 81.8(2) . . ?
O2 Cr3 Cl1 94.8(3) . . ?
O1 Cr3 Cl2 97.0(3) . . ?
O2 Cr3 Cl2 82.4(2) . . ?
Cl1 Cr3 Cl2 159.16(14) . . ?
O1 Cr3 Cr2 47.7(2) . . ?
O2 Cr3 Cr2 122.2(3) . . ?
Cl1 Cr3 Cr2 55.86(10) . . ?
Cl2 Cr3 Cr2 108.36(12) . . ?
O1 Cr3 Cr1 122.6(2) . . ?
O2 Cr3 Cr1 48.5(2) . . ?
Cl1 Cr3 Cr1 107.17(13) . . ?
Cl2 Cr3 Cr1 55.99(11) . . ?
Cr2 Cr3 Cr1 90.16(11) . . ?
Cr3 Cl2 Cr1 68.56(11) . . ?
Cr2 Cl1 Cr3 68.34(11) . . ?
O1 Si1 C5 105.0(5) . . ?
O1 Si1 C9 108.7(7) . . ?
C5 Si1 C9 122.2(7) . . ?
O1 Si1 C1 104.4(5) . . ?
C5 Si1 C1 108.7(6) . . ?
C9 Si1 C1 106.6(6) . . ?
O2 Si2 C21 110.5(5) . . ?
O2 Si2 C17 108.9(5) . . ?
C21 Si2 C17 115.5(6) . . ?
O2 Si2 C13 103.9(6) . . ?
C21 Si2 C13 110.0(6) . . ?
C17 Si2 C13 107.4(6) . . ?
Si1 O1 Cr2 136.2(5) . . ?
Si1 O1 Cr3 138.6(5) . . ?
Cr2 O1 Cr3 83.6(3) . . ?
Si2 O2 Cr3 134.8(5) . . ?
Si2 O2 Cr1 139.8(5) . . ?
Cr3 O2 Cr1 82.8(3) . . ?
C7 C5 C8 109.5(11) . . ?
C7 C5 C6 105.7(12) . . ?
C8 C5 C6 105.7(12) . . ?
C7 C5 Si1 115.2(10) . . ?
C8 C5 Si1 110.8(10) . . ?
C6 C5 Si1 109.5(11) . . ?
C23 C21 C24 112.7(10) . . ?
C23 C21 C22 106.4(12) . . ?
C24 C21 C22 105.8(11) . . ?
C23 C21 Si2 116.0(9) . . ?
C24 C21 Si2 115.6(9) . . ?
C22 C21 Si2 98.2(14) . . ?
C4 C1 C2 108.3(11) . . ?
C4 C1 C3 110.8(11) . . ?
C2 C1 C3 106.1(11) . . ?
C4 C1 Si1 114.6(9) . . ?
C2 C1 Si1 110.0(11) . . ?
C3 C1 Si1 106.7(10) . . ?
C19 C17 C20 112.1(12) . . ?
C19 C17 C18 109.0(12) . . ?
C20 C17 C18 107.1(11) . . ?
C19 C17 Si2 105.4(12) . . ?
C20 C17 Si2 116.3(10) . . ?
C18 C17 Si2 106.7(10) . . ?
C15 C13 C16 108.3(13) . . ?
C15 C13 C14 109.2(12) . . ?
C16 C13 C14 106.8(12) . . ?
C15 C13 Si2 116.9(12) . . ?
C16 C13 Si2 106.2(12) . . ?
C14 C13 Si2 109.1(11) . . ?
C10 C9 C12 112.8(12) . . ?
C10 C9 C11 105.5(14) . . ?
C12 C9 C11 102.1(12) . . ?
C10 C9 Si1 115.3(13) . . ?
C12 C9 Si1 124.7(13) . . ?
C11 C9 Si1 89.8(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 O2 2.027(8) . ?
Cr1 O2 2.027(8) 2 ?
Cr1 Cl2 2.393(4) . ?
Cr1 Cl2 2.394(4) 2 ?
Cr1 Cr3 2.687(3) . ?
Cr1 Cr3 2.688(3) 2 ?
Cr2 O1 1.987(8) . ?
Cr2 O1 1.987(8) 2 ?
Cr2 Cl1 2.378(3) . ?
Cr2 Cl1 2.378(3) 2 ?
Cr2 Cr3 2.670(3) . ?
Cr2 Cr3 2.670(3) 2 ?
Cr3 O1 2.016(8) . ?
Cr3 O2 2.036(8) . ?
Cr3 Cl1 2.376(4) . ?
Cr3 Cl2 2.378(4) . ?
Si1 O1 1.694(9) . ?
Si1 C5 1.894(11) . ?
Si1 C9 1.882(12) . ?
Si1 C1 2.004(11) . ?
Si2 O2 1.655(8) . ?
Si2 C21 1.888(11) . ?
Si2 C17 1.920(11) . ?
Si2 C13 1.985(11) . ?
C24 C21 1.516(14) . ?
C23 C21 1.500(13) . ?
C8 C5 1.548(15) . ?
C7 C5 1.535(15) . ?
C6 C5 1.578(15) . ?
C21 C22 1.604(15) . ?
C19 C17 1.516(15) . ?
C18 C17 1.553(15) . ?
C4 C1 1.513(13) . ?
C1 C2 1.548(14) . ?
C1 C3 1.552(15) . ?
C17 C20 1.524(14) . ?
C15 C13 1.516(15) . ?
C14 C13 1.557(15) . ?
C13 C16 1.557(16) . ?
C12 C9 1.520(16) . ?
C11 C9 1.628(17) . ?
C10 C9 1.491(16) . ?
