#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075410.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_4075410
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 Tm'
_chemical_formula_weight         638.37
_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                 108.892(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.942(3)
_cell_length_b                   11.358(2)
_cell_length_c                   16.952(3)
_cell_measurement_reflns_used    728
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2904.1(9)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0189
_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            19421
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.248
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.500096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00004(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.551
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.551
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.246
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+10.2390P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                5026
_reflns_number_total             5100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060268ksi20060525_065827.cif
_cod_data_source_block           C14_hos227
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075410
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
Tm Tm 0.419957(15) 0.13640(2) 0.946700(14) 0.02567(10) Uani 1 1 d .
Cl Cl 0.37944(11) 0.33247(13) 0.99716(10) 0.0440(4) Uani 1 1 d .
Si1 Si 0.82958(11) -0.09718(18) 1.01921(11) 0.0420(4) Uani 1 1 d .
Si2 Si 0.62367(12) -0.13621(17) 0.82441(10) 0.0393(4) Uani 1 1 d .
C1 C 0.7126(4) -0.0507(5) 1.0049(3) 0.0304(12) Uani 1 1 d .
C2 C 0.6342(3) -0.0656(5) 0.9281(3) 0.0275(12) Uani 1 1 d .
B3 B 0.5568(4) 0.0179(6) 0.9285(4) 0.0267(13) Uani 1 1 d .
H3 H 0.5092 0.0113 0.8643 0.07(2) Uiso 1 1 calc R
B4 B 0.5926(4) 0.0949(6) 1.0163(4) 0.0271(13) Uani 1 1 d .
H4 H 0.5870 0.1750 1.0518 0.09(3) Uiso 1 1 calc R
B5 B 0.6932(4) 0.0425(6) 1.0639(4) 0.0294(14) Uani 1 1 d .
H5 H 0.7406 0.0766 1.1230 0.030(15) Uiso 1 1 calc R
B6 B 0.6672(4) 0.0764(6) 0.9567(4) 0.0310(14) Uani 1 1 d .
H6 H 0.6950 0.1452 0.9258 0.039(16) Uiso 1 1 calc R
O11 O 0.4810(3) 0.2753(3) 0.8695(2) 0.0350(9) Uani 1 1 d .
C12 C 0.5357(5) 0.3763(6) 0.9082(4) 0.0536(19) Uani 1 1 d .
H12A H 0.5875 0.3506 0.9543 0.08(3) Uiso 1 1 calc R
H12B H 0.5015 0.4318 0.9299 0.05(2) Uiso 1 1 calc R
C13 C 0.5642(5) 0.4332(6) 0.8409(5) 0.0535(18) Uani 1 1 d .
H13A H 0.6241 0.4660 0.8636 0.07(2) Uiso 1 1 calc R
H13B H 0.5231 0.4959 0.8130 0.07(2) Uiso 1 1 calc R
C14 C 0.5617(5) 0.3321(6) 0.7816(4) 0.0503(17) Uani 1 1 d .
H14A H 0.5533 0.3607 0.7250 0.06(2) Uiso 1 1 calc R
H14B H 0.6162 0.2852 0.8006 0.06(2) Uiso 1 1 calc R
C15 C 0.4832(5) 0.2623(6) 0.7851(4) 0.0425(15) Uani 1 1 d .
H15A H 0.4285 0.2928 0.7449 0.08(3) Uiso 1 1 calc R
H15B H 0.4896 0.1793 0.7725 0.026(15) Uiso 1 1 calc R
O21 O 0.3271(2) 0.1287(3) 0.8094(2) 0.0319(9) Uani 1 1 d .
C22 C 0.3142(4) 0.0318(5) 0.7498(3) 0.0338(13) Uani 1 1 d .
H22A H 0.3263 -0.0442 0.7786 0.022(14) Uiso 1 1 calc R
H22B H 0.3532 0.0406 0.7157 0.045(18) Uiso 1 1 calc R
C23 C 0.2181(4) 0.0410(6) 0.6966(4) 0.0435(16) Uani 1 1 d .
H23A H 0.2081 0.0074 0.6411 0.040(17) Uiso 1 1 calc R
H23B H 0.1794 0.0015 0.7230 0.047(19) Uiso 1 1 calc R
C24 C 0.2034(5) 0.1716(6) 0.6923(4) 0.0519(19) Uani 1 1 d .
H24A H 0.2244 0.2070 0.6494 0.06(2) Uiso 1 1 calc R
H24B H 0.1404 0.1902 0.6798 0.10(3) Uiso 1 1 calc R
C25 C 0.2559(4) 0.2148(6) 0.7765(4) 0.0460(17) Uani 1 1 d .
H25A H 0.2806 0.2929 0.7730 0.06(2) Uiso 1 1 calc R
H25B H 0.2188 0.2198 0.8125 0.06(2) Uiso 1 1 calc R
O31 O 0.8858(7) 0.3665(11) 1.0911(5) 0.151(4) Uani 1 1 d .
C32 C 0.9485(12) 0.337(2) 1.0627(8) 0.157(7) Uani 1 1 d .
H32A H 0.9722 0.2601 1.0846 0.35(15) Uiso 1 1 calc R
H32B H 0.9968 0.3950 1.0807 0.35(16) Uiso 1 1 calc R
C33 C 0.9127(10) 0.333(2) 0.9696(7) 0.136(6) Uani 1 1 d .
H33A H 0.9511 0.3773 0.9451 0.30(12) Uiso 1 1 calc R
H33B H 0.9079 0.2520 0.9496 0.33(15) Uiso 1 1 calc R
C34 C 0.8273(7) 0.3870(15) 0.9487(7) 0.106(4) Uani 1 1 d .
H34A H 0.7841 0.3438 0.9034 0.19(7) Uiso 1 1 calc R
H34B H 0.8295 0.4688 0.9311 0.19(8) Uiso 1 1 calc R
C35 C 0.8030(9) 0.3816(18) 1.0259(7) 0.132(5) Uani 1 1 d .
H35A H 0.7738 0.4545 1.0338 0.23(10) Uiso 1 1 calc R
H35B H 0.7633 0.3151 1.0242 2.0(15) Uiso 1 1 calc R
C101 C 0.8475(5) -0.2591(7) 1.0317(5) 0.060(2) Uani 1 1 d .
H10A H 0.8093 -0.2991 0.9827 0.05(2) Uiso 1 1 calc R
H10B H 0.8337 -0.2855 1.0806 0.13(4) Uiso 1 1 calc R
H10C H 0.9090 -0.2771 1.0385 0.10(3) Uiso 1 1 calc R
C102 C 0.8674(5) -0.0418(8) 0.9327(5) 0.059(2) Uani 1 1 d .
H10D H 0.8600 0.0429 0.9282 0.05(2) Uiso 1 1 calc R
H10E H 0.8325 -0.0783 0.8807 0.07(3) Uiso 1 1 calc R
H10F H 0.9295 -0.0614 0.9442 0.12(4) Uiso 1 1 calc R
C103 C 0.9052(4) -0.0286(8) 1.1168(5) 0.057(2) Uani 1 1 d .
H10G H 0.9001 0.0564 1.1126 0.06(2) Uiso 1 1 calc R
H10H H 0.9659 -0.0515 1.1243 0.08(3) Uiso 1 1 calc R
H10I H 0.8889 -0.0553 1.1642 0.07(3) Uiso 1 1 calc R
C201 C 0.7002(5) -0.2601(7) 0.8234(5) 0.057(2) Uani 1 1 d .
H20A H 0.6941 -0.3217 0.8608 0.07(3) Uiso 1 1 calc R
H20B H 0.7608 -0.2316 0.8416 0.09(3) Uiso 1 1 calc R
H20C H 0.6855 -0.2913 0.7673 0.09(3) Uiso 1 1 calc R
C202 C 0.5098(5) -0.2003(8) 0.7828(5) 0.060(2) Uani 1 1 d .
H20D H 0.5028 -0.2610 0.8205 0.14(5) Uiso 1 1 calc R
H20E H 0.5013 -0.2342 0.7283 0.07(2) Uiso 1 1 calc R
H20F H 0.4662 -0.1388 0.7782 0.09(3) Uiso 1 1 calc R
C203 C 0.6364(7) -0.0182(8) 0.7520(5) 0.070(3) Uani 1 1 d .
H20G H 0.6952 0.0161 0.7739 0.10(4) Uiso 1 1 calc R
H20H H 0.5922 0.0425 0.7472 0.09(3) Uiso 1 1 calc R
H20I H 0.6285 -0.0519 0.6975 0.13(4) 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'
Tm Tm -0.3139 5.2483 '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 Tm O11 73.91(13) . .
O21 Tm Cl 102.79(10) . .
O11 Tm Cl 78.67(10) . .
O21 Tm C2 121.44(15) . 3_657
O11 Tm C2 155.56(15) . 3_657
Cl Tm C2 79.23(12) . 3_657
O21 Tm B4 132.10(16) . .
O11 Tm B4 79.50(17) . .
Cl Tm B4 110.16(14) . .
C2 Tm B4 98.56(18) 3_657 .
O21 Tm B3 98.37(16) . .
O11 Tm B3 77.36(16) . .
Cl Tm B3 141.99(14) . .
C2 Tm B3 115.38(17) 3_657 .
B4 Tm B3 36.32(18) . .
O21 Tm B3 130.34(17) . 3_657
O11 Tm B3 150.21(16) . 3_657
Cl Tm B3 107.01(14) . 3_657
C2 Tm B3 33.93(17) 3_657 3_657
B4 Tm B3 71.05(19) . 3_657
B3 Tm B3 81.46(19) . 3_657
O21 Tm B5 72.96(17) . 3_657
O11 Tm B5 145.90(16) . 3_657
Cl Tm B5 116.56(15) . 3_657
C2 Tm B5 55.96(18) 3_657 3_657
B4 Tm B5 118.2(2) . 3_657
B3 Tm B5 99.6(2) . 3_657
B3 Tm B5 58.40(19) 3_657 3_657
O21 Tm C1 89.03(16) . 3_657
O11 Tm C1 152.49(16) . 3_657
Cl Tm C1 84.48(13) . 3_657
C2 Tm C1 32.43(16) 3_657 3_657
B4 Tm C1 127.11(18) . 3_657
B3 Tm C1 127.37(18) . 3_657
B3 Tm C1 56.14(18) 3_657 3_657
B5 Tm C1 33.68(18) 3_657 3_657
O21 Tm B4 97.10(16) . 3_657
O11 Tm B4 144.84(16) . 3_657
Cl Tm B4 136.20(13) . 3_657
C2 Tm B4 57.17(17) 3_657 3_657
B4 Tm B4 82.5(2) . 3_657
B3 Tm B4 70.32(18) . 3_657
B3 Tm B4 35.79(18) 3_657 3_657
B5 Tm B4 35.64(18) 3_657 3_657
C1 Tm B4 57.05(18) 3_657 3_657
C101 Si1 C102 110.2(4) . .
C101 Si1 C103 106.2(4) . .
C102 Si1 C103 106.0(4) . .
C101 Si1 C1 113.7(3) . .
C102 Si1 C1 111.4(3) . .
C103 Si1 C1 109.0(3) . .
C201 Si2 C202 105.1(4) . .
C201 Si2 C203 108.9(4) . .
C202 Si2 C203 109.3(4) . .
C201 Si2 C2 117.8(3) . .
C202 Si2 C2 107.4(3) . .
C203 Si2 C2 108.0(3) . .
C2 C1 B5 110.7(5) . .
C2 C1 B6 64.6(4) . .
B5 C1 B6 65.7(4) . .
C2 C1 Si1 126.6(4) . .
B5 C1 Si1 120.3(4) . .
B6 C1 Si1 123.5(4) . .
C2 C1 Tm 72.9(3) . 3_657
B5 C1 Tm 73.2(3) . 3_657
B6 C1 Tm 101.5(3) . 3_657
Si1 C1 Tm 134.9(3) . 3_657
C1 C2 B3 111.6(5) . .
C1 C2 B6 63.6(4) . .
B3 C2 B6 66.3(4) . .
C1 C2 Si2 131.0(4) . .
B3 C2 Si2 115.5(4) . .
B6 C2 Si2 126.1(4) . .
C1 C2 Tm 74.6(3) . 3_657
B3 C2 Tm 73.6(3) . 3_657
B6 C2 Tm 101.9(3) . 3_657
Si2 C2 Tm 131.2(3) . 3_657
C2 B3 B4 106.4(5) . .
C2 B3 B6 61.1(4) . .
B4 B3 B6 62.8(4) . .
C2 B3 Tm 170.9(4) . .
B4 B3 Tm 71.8(3) . .
B6 B3 Tm 123.4(4) . .
C2 B3 Tm 72.5(3) . 3_657
B4 B3 Tm 73.6(3) . 3_657
B6 B3 Tm 99.2(3) . 3_657
Tm B3 Tm 98.54(19) . 3_657
B5 B4 B3 104.2(5) . .
B5 B4 B6 61.4(4) . .
B3 B4 B6 62.3(3) . .
B5 B4 Tm 168.3(4) . .
B3 B4 Tm 71.9(3) . .
B6 B4 Tm 123.1(4) . .
B5 B4 Tm 70.9(3) . 3_657
B3 B4 Tm 70.6(3) . 3_657
B6 B4 Tm 97.3(3) . 3_657
Tm B4 Tm 97.5(2) . 3_657
C1 B5 B4 107.1(5) . .
C1 B5 B6 61.1(4) . .
B4 B5 B6 63.4(4) . .
C1 B5 Tm 73.2(3) . 3_657
B4 B5 Tm 73.5(3) . 3_657
B6 B5 Tm 99.6(3) . 3_657
C1 B6 C2 51.8(3) . .
C1 B6 B5 53.2(3) . .
C2 B6 B5 92.0(4) . .
C1 B6 B3 92.4(4) . .
C2 B6 B3 52.6(3) . .
B5 B6 B3 94.4(4) . .
C1 B6 B4 94.9(4) . .
C2 B6 B4 94.1(4) . .
B5 B6 B4 55.2(3) . .
B3 B6 B4 54.9(3) . .
C15 O11 C12 108.8(5) . .
C15 O11 Tm 127.1(3) . .
C12 O11 Tm 123.3(3) . .
O11 C12 C13 106.2(5) . .
C12 C13 C14 103.2(6) . .
C15 C14 C13 102.5(6) . .
O11 C15 C14 105.8(5) . .
C22 O21 C25 108.7(4) . .
C22 O21 Tm 128.5(3) . .
C25 O21 Tm 121.4(3) . .
O21 C22 C23 104.4(5) . .
C24 C23 C22 102.2(5) . .
C25 C24 C23 104.4(5) . .
O21 C25 C24 105.8(5) . .
C32 O31 C35 112.2(10) . .
O31 C32 C33 109.0(12) . .
C34 C33 C32 104.8(12) . .
C33 C34 C35 105.3(11) . .
O31 C35 C34 104.3(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tm O21 2.320(4) .
Tm O11 2.445(4) .
Tm Cl 2.5427(15) .
Tm C2 2.662(5) 3_657
Tm B4 2.662(6) .
Tm B3 2.665(6) .
Tm B3 2.678(6) 3_657
Tm B5 2.685(6) 3_657
Tm C1 2.685(6) 3_657
Tm B4 2.723(7) 3_657
Si1 C101 1.863(8) .
Si1 C102 1.867(7) .
Si1 C103 1.873(7) .
Si1 C1 1.877(6) .
Si2 C201 1.866(7) .
Si2 C202 1.869(8) .
Si2 C203 1.872(8) .
Si2 C2 1.889(6) .
C1 C2 1.493(7) .
C1 B5 1.556(9) .
C1 B6 1.701(9) .
C1 Tm 2.685(6) 3_657
C2 B3 1.558(8) .
C2 B6 1.717(8) .
C2 Tm 2.662(5) 3_657
B3 B4 1.660(8) .
B3 B6 1.795(9) .
B3 Tm 2.678(6) 3_657
B4 B5 1.656(9) .
B4 B6 1.804(9) .
B4 Tm 2.723(6) 3_657
B5 B6 1.771(9) .
B5 Tm 2.685(6) 3_657
O11 C15 1.449(7) .
O11 C12 1.462(7) .
C12 C13 1.502(9) .
C13 C14 1.519(10) .
C14 C15 1.500(9) .
O21 C22 1.463(6) .
O21 C25 1.464(7) .
C22 C23 1.509(8) .
C23 C24 1.499(9) .
C24 C25 1.485(9) .
O31 C32 1.284(15) .
O31 C35 1.431(15) .
C32 C33 1.496(16) .
C33 C34 1.428(15) .
C34 C35 1.482(14) .
