#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075402.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_4075402
loop_
_publ_author_name
'Wang, Jianhui'
'Smith, Joanna'
'Zheng, Chong'
'Maguire, John A.'
'Hosmane, Narayan S.'
_publ_section_title
;
 Chemistry of C-Trimethylsilyl-Substituted Heterocarboranes. 32. Synthetic
 and Structural Investigations on Half-Sandwich
 Lanthanacarboranes:  Important Synthons in Metallacarborane
 Chemistry
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4118
_journal_paper_doi               10.1021/om060268k
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C20 H46 B4 Cl O3 Si2 Y'
_chemical_formula_weight         558.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.887(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.956(3)
_cell_length_b                   11.396(2)
_cell_length_c                   16.968(4)
_cell_measurement_reflns_used    614
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2919.2(10)
_computing_cell_refinement       'SMART and SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      208(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Siemens SMART CCD  PLATFORM'
_diffrn_measurement_method       'ω 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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17584
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.082162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0000(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.322
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.322
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          4.743
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0130P)²+12.3572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                4105
_reflns_number_total             4981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060268ksi20060525_065827.cif
_cod_data_source_block           C3_hos242
_cod_original_cell_volume        2919.2(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075402
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Y Y 0.41951(4) 0.13851(5) 0.94621(3) 0.02248(18) Uani 1 1 d .
Cl Cl 0.38023(12) 0.33544(13) 0.99882(11) 0.0434(4) Uani 1 1 d .
Si1 Si 0.83033(12) -0.09774(18) 1.01897(12) 0.0406(5) Uani 1 1 d .
Si2 Si 0.62451(12) -0.13503(17) 0.82405(11) 0.0381(4) Uani 1 1 d .
C1 C 0.7132(4) -0.0500(5) 1.0043(3) 0.0268(13) Uani 1 1 d .
C2 C 0.6347(4) -0.0644(5) 0.9271(3) 0.0253(13) Uani 1 1 d .
B3 B 0.5587(4) 0.0190(5) 0.9286(4) 0.0216(14) Uani 1 1 d .
H3 H 0.5113 0.0132 0.8643 0.035(17) Uiso 1 1 calc R
B4 B 0.5945(4) 0.0945(6) 1.0165(4) 0.0245(14) Uani 1 1 d .
H4 H 0.5894 0.1740 1.0525 0.09(3) Uiso 1 1 calc R
B5 B 0.6949(4) 0.0424(6) 1.0649(4) 0.0268(15) Uani 1 1 d .
H5 H 0.7422 0.0758 1.1240 0.037(17) Uiso 1 1 calc R
B6 B 0.6676(5) 0.0773(6) 0.9559(4) 0.0296(16) Uani 1 1 d .
H6 H 0.6950 0.1460 0.9248 0.036(16) Uiso 1 1 calc R
O11 O 0.4803(3) 0.2783(3) 0.8677(2) 0.0350(10) Uani 1 1 d .
C12 C 0.5348(5) 0.3786(6) 0.9059(5) 0.052(2) Uani 1 1 d .
H12A H 0.5860 0.3533 0.9527 0.08(3) Uiso 1 1 calc R
H12B H 0.5003 0.4350 0.9265 0.09(3) Uiso 1 1 calc R
C13 C 0.5642(6) 0.4326(6) 0.8389(5) 0.056(2) Uani 1 1 d .
H13A H 0.6242 0.4649 0.8618 0.06(2) Uiso 1 1 calc R
H13B H 0.5237 0.4952 0.8101 0.07(3) Uiso 1 1 calc R
C14 C 0.5620(5) 0.3317(6) 0.7812(4) 0.0476(18) Uani 1 1 d .
H14A H 0.5548 0.3592 0.7247 0.049(19) Uiso 1 1 calc R
H14B H 0.6161 0.2843 0.8013 0.05(2) Uiso 1 1 calc R
C15 C 0.4827(5) 0.2637(6) 0.7837(4) 0.0417(17) Uani 1 1 d .
H15A H 0.4286 0.2946 0.7431 0.05(2) Uiso 1 1 calc R
H15B H 0.4887 0.1806 0.7716 0.06(2) Uiso 1 1 calc R
O21 O 0.3253(3) 0.1289(3) 0.8078(2) 0.0311(9) Uani 1 1 d .
C22 C 0.3130(4) 0.0325(5) 0.7479(4) 0.0344(15) Uani 1 1 d .
H22A H 0.3260 -0.0434 0.7765 0.025(15) Uiso 1 1 calc R
H22B H 0.3514 0.0424 0.7134 0.042(19) Uiso 1 1 calc R
C23 C 0.2178(4) 0.0406(6) 0.6963(4) 0.0418(17) Uani 1 1 d .
H23A H 0.1799 0.0018 0.7237 0.039(18) Uiso 1 1 calc R
H23B H 0.2073 0.0054 0.6412 0.044(19) Uiso 1 1 calc R
C24 C 0.2015(5) 0.1709(6) 0.6898(5) 0.052(2) Uani 1 1 d .
H24A H 0.2218 0.2056 0.6463 0.08(3) Uiso 1 1 calc R
H24B H 0.1385 0.1888 0.6778 0.07(2) Uiso 1 1 calc R
C25 C 0.2550(5) 0.2141(6) 0.7741(4) 0.0466(18) Uani 1 1 d .
H25A H 0.2801 0.2915 0.7700 0.047(19) Uiso 1 1 calc R
H25B H 0.2180 0.2206 0.8101 0.05(2) Uiso 1 1 calc R
O31 O 0.8866(7) 0.3666(10) 1.0911(5) 0.148(4) Uani 1 1 d .
C32 C 0.9478(13) 0.336(2) 1.0616(8) 0.169(8) Uani 1 1 d .
H32A H 0.9707 0.2588 1.0830 0.33(14) Uiso 1 1 calc R
H32B H 0.9968 0.3927 1.0792 0.36(18) Uiso 1 1 calc R
C33 C 0.9111(10) 0.333(2) 0.9689(8) 0.151(6) Uani 1 1 d .
H33A H 0.9493 0.3768 0.9441 0.21(8) Uiso 1 1 calc R
H33B H 0.9059 0.2520 0.9486 0.34(16) Uiso 1 1 calc R
C34 C 0.8272(8) 0.3861(17) 0.9490(7) 0.114(5) Uani 1 1 d .
H34A H 0.7836 0.3428 0.9043 0.18(6) Uiso 1 1 calc R
H34B H 0.8295 0.4672 0.9307 0.23(10) Uiso 1 1 calc R
C35 C 0.8031(10) 0.3830(17) 1.0257(8) 0.135(5) Uani 1 1 d .
H35A H 0.7750 0.4567 1.0333 0.6(3) Uiso 1 1 calc R
H35B H 0.7625 0.3180 1.0244 2.0(16) Uiso 1 1 calc R
C101 C 0.8472(5) -0.2604(7) 1.0315(6) 0.062(2) Uani 1 1 d .
H10A H 0.8089 -0.2998 0.9824 0.12(4) Uiso 1 1 calc R
H10B H 0.8330 -0.2864 1.0801 0.12(4) Uiso 1 1 calc R
H10C H 0.9085 -0.2791 1.0384 0.12(4) Uiso 1 1 calc R
C102 C 0.8687(5) -0.0427(8) 0.9323(5) 0.060(2) Uani 1 1 d .
H10D H 0.8614 0.0418 0.9277 0.09(3) Uiso 1 1 calc R
H10E H 0.8339 -0.0792 0.8804 0.07(3) Uiso 1 1 calc R
H10F H 0.9307 -0.0623 0.9440 0.10(3) Uiso 1 1 calc R
C103 C 0.9062(5) -0.0308(8) 1.1167(5) 0.056(2) Uani 1 1 d .
H10G H 0.9014 0.0541 1.1129 0.06(2) Uiso 1 1 calc R
H10H H 0.9668 -0.0539 1.1239 0.07(2) Uiso 1 1 calc R
H10I H 0.8899 -0.0577 1.1639 0.07(3) Uiso 1 1 calc R
C201 C 0.7007(5) -0.2596(7) 0.8227(5) 0.056(2) Uani 1 1 d .
H20A H 0.6944 -0.3209 0.8601 0.06(2) Uiso 1 1 calc R
H20B H 0.7614 -0.2317 0.8407 0.08(3) Uiso 1 1 calc R
H20C H 0.6857 -0.2907 0.7666 0.10(3) Uiso 1 1 calc R
C202 C 0.5108(5) -0.1982(8) 0.7821(5) 0.059(2) Uani 1 1 d .
H20D H 0.5035 -0.2589 0.8195 0.09(3) Uiso 1 1 calc R
H20E H 0.5023 -0.2318 0.7276 0.08(3) Uiso 1 1 calc R
H20F H 0.4674 -0.1368 0.7776 0.09(3) Uiso 1 1 calc R
C203 C 0.6379(7) -0.0172(8) 0.7523(5) 0.070(3) Uani 1 1 d .
H20G H 0.6967 0.0166 0.7745 0.13(5) Uiso 1 1 calc R
H20H H 0.5938 0.0434 0.7475 0.10(4) Uiso 1 1 calc R
H20I H 0.6302 -0.0505 0.6978 0.09(3) 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'
B B 0.0013 0.0007 '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'
Y Y -2.7962 3.5667 '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'
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
O21 Y O11 74.11(14) . .
O21 Y Cl 103.86(10) . .
O11 Y Cl 78.83(11) . .
O21 Y C2 121.07(16) . 3_657
O11 Y C2 156.23(15) . 3_657
Cl Y C2 79.60(13) . 3_657
O21 Y B3 98.55(16) . .
O11 Y B3 77.57(16) . .
Cl Y B3 141.35(14) . .
C2 Y B3 114.64(17) 3_657 .
O21 Y B4 131.95(17) . .
O11 Y B4 80.07(17) . .
Cl Y B4 110.01(14) . .
C2 Y B4 98.15(18) 3_657 .
B3 Y B4 35.67(18) . .
O21 Y C1 88.92(16) . 3_657
O11 Y C1 152.86(16) . 3_657
Cl Y C1 85.09(13) . 3_657
C2 Y C1 32.17(17) 3_657 3_657
B3 Y C1 126.77(18) . 3_657
B4 Y C1 126.32(18) . 3_657
O21 Y B3 129.10(17) . 3_657
O11 Y B3 151.10(17) . 3_657
Cl Y B3 106.83(14) . 3_657
C2 Y B3 33.19(18) 3_657 3_657
B3 Y B3 81.48(19) . 3_657
B4 Y B3 71.32(19) . 3_657
C1 Y B3 55.06(18) 3_657 3_657
O21 Y B5 72.36(17) . 3_657
O11 Y B5 145.52(17) . 3_657
Cl Y B5 116.94(15) . 3_657
C2 Y B5 55.74(18) 3_657 3_657
B3 Y B5 99.6(2) . 3_657
B4 Y B5 117.6(2) . 3_657
C1 Y B5 33.48(19) 3_657 3_657
B3 Y B5 57.75(19) 3_657 3_657
O21 Y B4 96.41(17) . 3_657
O11 Y B4 145.20(17) . 3_657
Cl Y B4 135.70(14) . 3_657
C2 Y B4 56.28(18) 3_657 3_657
B3 Y B4 70.75(19) . 3_657
B4 Y B4 82.5(2) . 3_657
C1 Y B4 56.04(18) 3_657 3_657
B3 Y B4 35.22(18) 3_657 3_657
B5 Y B4 35.2(2) 3_657 3_657
C103 Si1 C102 106.1(4) . .
C103 Si1 C101 106.0(4) . .
C102 Si1 C101 110.3(4) . .
C103 Si1 C1 109.2(3) . .
C102 Si1 C1 111.2(3) . .
C101 Si1 C1 113.6(3) . .
C202 Si2 C203 109.3(5) . .
C202 Si2 C201 104.9(4) . .
C203 Si2 C201 109.0(4) . .
C202 Si2 C2 107.4(3) . .
C203 Si2 C2 107.7(3) . .
C201 Si2 C2 118.3(3) . .
C2 C1 B5 111.4(5) . .
C2 C1 B6 64.4(4) . .
B5 C1 B6 66.6(4) . .
C2 C1 Si1 126.7(4) . .
B5 C1 Si1 119.7(4) . .
B6 C1 Si1 124.0(4) . .
C2 C1 Y 73.4(3) . 3_657
B5 C1 Y 73.5(3) . 3_657
B6 C1 Y 102.1(3) . 3_657
Si1 C1 Y 133.8(3) . 3_657
C1 C2 B3 110.9(5) . .
C1 C2 B6 63.7(4) . .
B3 C2 B6 65.7(4) . .
C1 C2 Si2 130.8(4) . .
B3 C2 Si2 116.4(4) . .
B6 C2 Si2 126.3(4) . .
C1 C2 Y 74.5(3) . 3_657
B3 C2 Y 74.0(3) . 3_657
B6 C2 Y 102.4(3) . 3_657
Si2 C2 Y 130.7(3) . 3_657
C2 B3 B4 106.8(5) . .
C2 B3 B6 61.8(4) . .
B4 B3 B6 63.1(4) . .
C2 B3 Y 170.9(4) . .
B4 B3 Y 72.2(3) . .
B6 B3 Y 123.5(4) . .
C2 B3 Y 72.8(3) . 3_657
B4 B3 Y 73.7(3) . 3_657
B6 B3 Y 100.1(3) . 3_657
Y B3 Y 98.52(19) . 3_657
B5 B4 B3 104.9(5) . .
B5 B4 B6 62.7(4) . .
B3 B4 B6 61.7(4) . .
B5 B4 Y 168.6(4) . .
B3 B4 Y 72.1(3) . .
B6 B4 Y 122.4(4) . .
B5 B4 Y 71.2(3) . 3_657
B3 B4 Y 71.1(3) . 3_657
B6 B4 Y 98.1(3) . 3_657
Y B4 Y 97.5(2) . 3_657
C1 B5 B4 105.8(5) . .
C1 B5 B6 60.5(4) . .
B4 B5 B6 62.5(4) . .
C1 B5 Y 73.1(3) . 3_657
B4 B5 Y 73.6(3) . 3_657
B6 B5 Y 99.3(3) . 3_657
C1 B6 C2 51.9(3) . .
C1 B6 B3 92.1(4) . .
C2 B6 B3 52.5(3) . .
C1 B6 B4 94.2(4) . .
C2 B6 B4 94.0(4) . .
B3 B6 B4 55.2(3) . .
C1 B6 B5 52.9(4) . .
C2 B6 B5 92.0(4) . .
B3 B6 B5 94.4(4) . .
B4 B6 B5 54.8(4) . .
C15 O11 C12 109.1(5) . .
C15 O11 Y 126.7(3) . .
C12 O11 Y 123.3(4) . .
O11 C12 C13 105.9(6) . .
C12 C13 C14 103.5(6) . .
C15 C14 C13 102.7(6) . .
O11 C15 C14 105.1(5) . .
C25 O21 C22 108.3(4) . .
C25 O21 Y 121.7(4) . .
C22 O21 Y 128.9(3) . .
O21 C22 C23 104.1(5) . .
C22 C23 C24 102.9(5) . .
C25 C24 C23 102.9(6) . .
O21 C25 C24 106.6(5) . .
C32 O31 C35 111.4(11) . .
O31 C32 C33 109.3(13) . .
C34 C33 C32 105.1(13) . .
C33 C34 C35 106.2(12) . .
O31 C35 C34 104.1(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Y O21 2.345(4) .
Y O11 2.468(4) .
Y Cl 2.5667(16) .
Y C2 2.698(5) 3_657
Y B3 2.703(7) .
Y B4 2.704(7) .
Y C1 2.714(6) 3_657
Y B3 2.716(6) 3_657
Y B5 2.720(6) 3_657
Y B4 2.755(6) 3_657
Si1 C103 1.870(7) .
Si1 C102 1.875(8) .
Si1 C101 1.875(8) .
Si1 C1 1.883(6) .
Si2 C202 1.866(7) .
Si2 C203 1.870(8) .
Si2 C201 1.874(7) .
Si2 C2 1.884(6) .
C1 C2 1.500(8) .
C1 B5 1.565(9) .
C1 B6 1.708(9) .
C1 Y 2.714(6) 3_657
C2 B3 1.547(9) .
C2 B6 1.719(8) .
C2 Y 2.698(5) 3_657
B3 B4 1.656(9) .
B3 B6 1.777(9) .
B3 Y 2.716(6) 3_657
B4 B5 1.656(9) .
B4 B6 1.798(9) .
B4 Y 2.755(6) 3_657
B5 B6 1.801(9) .
B5 Y 2.720(6) 3_657
O11 C15 1.447(7) .
O11 C12 1.455(7) .
C12 C13 1.497(10) .
C13 C14 1.504(10) .
C14 C15 1.496(9) .
O21 C25 1.454(7) .
O21 C22 1.467(7) .
C22 C23 1.491(8) .
C23 C24 1.506(9) .
C24 C25 1.493(9) .
O31 C32 1.280(15) .
O31 C35 1.444(15) .
C32 C33 1.492(17) .
C33 C34 1.408(15) .
C34 C35 1.471(14) .
