#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075406.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_4075406
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 Tb'
_chemical_formula_weight         628.36
_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                 108.972(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.966(3)
_cell_length_b                   11.432(2)
_cell_length_c                   17.002(4)
_cell_measurement_reflns_used    671
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2934.7(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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0226
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18372
_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    2.601
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.517117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.941
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.00030(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   1.541
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.541
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0084P)²+15.8232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                5005
_reflns_number_total             5088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060268ksi20060525_065827.cif
_cod_data_source_block           C10_hos226
_cod_original_cell_volume        2934.6(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075406
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
Tb Tb 0.41896(2) 0.13936(3) 0.946267(19) 0.02589(12) Uani 1 1 d .
Cl Cl 0.38164(14) 0.33705(16) 1.00125(13) 0.0457(5) Uani 1 1 d .
Si1 Si 0.83118(14) -0.0986(2) 1.01922(14) 0.0426(5) Uani 1 1 d .
Si2 Si 0.62511(14) -0.1336(2) 0.82374(12) 0.0398(5) Uani 1 1 d .
C1 C 0.7148(4) -0.0500(6) 1.0047(4) 0.0301(15) Uani 1 1 d .
C2 C 0.6353(4) -0.0647(6) 0.9274(4) 0.0294(15) Uani 1 1 d .
B3 B 0.5587(5) 0.0183(7) 0.9282(4) 0.0255(15) Uani 1 1 d .
H3 H 0.5113 0.0121 0.8640 0.06(3) Uiso 1 1 calc R
B4 B 0.5946(5) 0.0948(7) 1.0160(5) 0.0288(16) Uani 1 1 d .
H4 H 0.5892 0.1745 1.0513 0.11(4) Uiso 1 1 calc R
B5 B 0.6950(5) 0.0420(7) 1.0636(5) 0.0291(17) Uani 1 1 d .
H5 H 0.7423 0.0755 1.1227 0.033(19) Uiso 1 1 calc R
B6 B 0.6690(5) 0.0770(7) 0.9569(5) 0.0327(17) Uani 1 1 d .
H6 H 0.6969 0.1458 0.9265 0.04(2) Uiso 1 1 calc R
O11 O 0.4791(3) 0.2797(4) 0.8668(3) 0.0346(11) Uani 1 1 d .
C12 C 0.5340(6) 0.3806(7) 0.9053(5) 0.053(2) Uani 1 1 d .
H12A H 0.5848 0.3556 0.9525 0.07(3) Uiso 1 1 calc R
H12B H 0.4994 0.4374 0.9250 0.06(3) Uiso 1 1 calc R
C13 C 0.5645(6) 0.4334(8) 0.8380(5) 0.053(2) Uani 1 1 d .
H13A H 0.6247 0.4648 0.8612 0.06(3) Uiso 1 1 calc R
H13B H 0.5246 0.4963 0.8091 0.07(3) Uiso 1 1 calc R
C14 C 0.5619(6) 0.3318(8) 0.7798(5) 0.050(2) Uani 1 1 d .
H14A H 0.5544 0.3593 0.7234 0.05(2) Uiso 1 1 calc R
H14B H 0.6159 0.2845 0.7997 0.08(3) Uiso 1 1 calc R
C15 C 0.4827(6) 0.2644(7) 0.7828(5) 0.0426(19) Uani 1 1 d .
H15A H 0.4287 0.2948 0.7417 0.10(4) Uiso 1 1 calc R
H15B H 0.4888 0.1815 0.7712 0.033(19) Uiso 1 1 calc R
O21 O 0.3234(3) 0.1288(4) 0.8058(3) 0.0335(11) Uani 1 1 d .
C22 C 0.3122(5) 0.0317(6) 0.7474(4) 0.0336(16) Uani 1 1 d .
H22A H 0.3261 -0.0432 0.7769 0.017(16) Uiso 1 1 calc R
H22B H 0.3504 0.0414 0.7129 0.04(2) Uiso 1 1 calc R
C23 C 0.2154(5) 0.0377(7) 0.6950(5) 0.047(2) Uani 1 1 d .
H23A H 0.2052 0.0027 0.6400 0.05(2) Uiso 1 1 calc R
H23B H 0.1779 -0.0016 0.7225 0.04(2) Uiso 1 1 calc R
C24 C 0.1986(6) 0.1675(7) 0.6886(5) 0.054(2) Uani 1 1 d .
H24A H 0.2180 0.2019 0.6447 0.09(4) Uiso 1 1 calc R
H24B H 0.1356 0.1845 0.6770 0.11(4) Uiso 1 1 calc R
C25 C 0.2524(6) 0.2131(7) 0.7722(5) 0.048(2) Uani 1 1 d .
H25A H 0.2768 0.2903 0.7669 0.07(3) Uiso 1 1 calc R
H25B H 0.2160 0.2199 0.8085 0.05(3) Uiso 1 1 calc R
O31 O 0.8870(9) 0.3671(14) 1.0910(6) 0.152(5) Uani 1 1 d .
C32 C 0.9465(16) 0.336(3) 1.0616(10) 0.175(10) Uani 1 1 d .
H32A H 0.9687 0.2587 1.0830 0.23(11) Uiso 1 1 calc R
H32B H 0.9960 0.3915 1.0793 0.4(3) Uiso 1 1 calc R
C33 C 0.9110(13) 0.333(3) 0.9692(9) 0.143(7) Uani 1 1 d .
H33A H 0.9498 0.3754 0.9449 0.24(12) Uiso 1 1 calc R
H33B H 0.9052 0.2518 0.9490 0.32(18) Uiso 1 1 calc R
C34 C 0.8270(9) 0.3873(19) 0.9488(9) 0.110(5) Uani 1 1 d .
H34A H 0.7830 0.3447 0.9042 0.21(10) Uiso 1 1 calc R
H34B H 0.8300 0.4681 0.9307 0.18(9) Uiso 1 1 calc R
C35 C 0.8037(14) 0.385(3) 1.0254(9) 0.150(8) Uani 1 1 d .
H35A H 0.7761 0.4584 1.0331 0.4(2) Uiso 1 1 calc R
H35B H 0.7626 0.3203 1.0240 0.6(4) Uiso 1 1 calc R
C101 C 0.8464(6) -0.2591(9) 1.0315(7) 0.062(3) Uani 1 1 d .
H10A H 0.8079 -0.2979 0.9822 0.10(4) Uiso 1 1 calc R
H10B H 0.8316 -0.2845 1.0798 0.10(4) Uiso 1 1 calc R
H10C H 0.9075 -0.2787 1.0388 0.13(5) Uiso 1 1 calc R
C102 C 0.8701(6) -0.0443(10) 0.9330(6) 0.062(3) Uani 1 1 d .
H10D H 0.8629 0.0399 0.9282 0.05(3) Uiso 1 1 calc R
H10E H 0.8354 -0.0808 0.8811 0.11(4) Uiso 1 1 calc R
H10F H 0.9321 -0.0640 0.9450 0.13(5) Uiso 1 1 calc R
C103 C 0.9069(5) -0.0312(10) 1.1168(6) 0.058(2) Uani 1 1 d .
H10G H 0.9019 0.0533 1.1128 0.06(3) Uiso 1 1 calc R
H10H H 0.9675 -0.0541 1.1243 0.05(2) Uiso 1 1 calc R
H10I H 0.8905 -0.0579 1.1640 0.08(3) Uiso 1 1 calc R
C201 C 0.7003(6) -0.2583(9) 0.8219(6) 0.058(2) Uani 1 1 d .
H20A H 0.6940 -0.3193 0.8592 0.09(4) Uiso 1 1 calc R
H20B H 0.7612 -0.2311 0.8397 0.09(4) Uiso 1 1 calc R
H20C H 0.6848 -0.2891 0.7658 0.09(4) Uiso 1 1 calc R
C202 C 0.5106(6) -0.1958(10) 0.7814(6) 0.063(3) Uani 1 1 d .
H20D H 0.5030 -0.2564 0.8185 0.13(6) Uiso 1 1 calc R
H20E H 0.5019 -0.2290 0.7268 0.05(2) Uiso 1 1 calc R
H20F H 0.4674 -0.1343 0.7770 0.11(5) Uiso 1 1 calc R
C203 C 0.6392(9) -0.0160(10) 0.7523(6) 0.072(3) Uani 1 1 d .
H20G H 0.6980 0.0174 0.7747 0.10(4) Uiso 1 1 calc R
H20H H 0.5952 0.0446 0.7473 0.10(4) Uiso 1 1 calc R
H20I H 0.6316 -0.0493 0.6979 0.14(5) 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'
Tb Tb -0.1723 4.1537 '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 Tb O11 73.88(16) . .
O21 Tb Cl 105.00(12) . .
O11 Tb Cl 78.90(12) . .
O21 Tb C2 120.95(19) . 3_657
O11 Tb C2 156.52(18) . 3_657
Cl Tb C2 79.50(15) . 3_657
O21 Tb B4 131.5(2) . .
O11 Tb B4 80.3(2) . .
Cl Tb B4 109.42(17) . .
C2 Tb B4 98.4(2) 3_657 .
O21 Tb B3 98.16(19) . .
O11 Tb B3 77.95(19) . .
Cl Tb B3 140.98(17) . .
C2 Tb B3 114.5(2) 3_657 .
B4 Tb B3 35.6(2) . .
O21 Tb B3 129.0(2) . 3_657
O11 Tb B3 151.3(2) . 3_657
Cl Tb B3 106.34(16) . 3_657
C2 Tb B3 33.2(2) 3_657 3_657
B4 Tb B3 71.4(2) . 3_657
B3 Tb B3 81.3(2) . 3_657
O21 Tb B5 72.7(2) . 3_657
O11 Tb B5 145.69(19) . 3_657
Cl Tb B5 117.30(18) . 3_657
C2 Tb B5 55.2(2) 3_657 3_657
B4 Tb B5 117.3(2) . 3_657
B3 Tb B5 99.3(2) . 3_657
B3 Tb B5 57.4(2) 3_657 3_657
O21 Tb C1 88.71(19) . 3_657
O11 Tb C1 152.51(19) . 3_657
Cl Tb C1 85.51(15) . 3_657
C2 Tb C1 32.28(19) 3_657 3_657
B4 Tb C1 126.6(2) . 3_657
B3 Tb C1 126.5(2) . 3_657
B3 Tb C1 55.3(2) 3_657 3_657
B5 Tb C1 33.1(2) 3_657 3_657
O21 Tb B4 96.31(19) . 3_657
O11 Tb B4 145.2(2) . 3_657
Cl Tb B4 135.53(17) . 3_657
C2 Tb B4 56.1(2) 3_657 3_657
B4 Tb B4 82.3(2) . 3_657
B3 Tb B4 70.4(2) . 3_657
B3 Tb B4 35.1(2) 3_657 3_657
B5 Tb B4 35.0(2) 3_657 3_657
C1 Tb B4 56.0(2) 3_657 3_657
C101 Si1 C103 106.5(5) . .
C101 Si1 C102 110.5(5) . .
C103 Si1 C102 106.0(4) . .
C101 Si1 C1 113.3(4) . .
C103 Si1 C1 108.7(4) . .
C102 Si1 C1 111.4(4) . .
C201 Si2 C203 108.8(5) . .
C201 Si2 C202 104.8(5) . .
C203 Si2 C202 109.3(6) . .
C201 Si2 C2 118.2(4) . .
C203 Si2 C2 108.3(4) . .
C202 Si2 C2 107.1(4) . .
C2 C1 B5 110.3(6) . .
C2 C1 B6 64.7(4) . .
B5 C1 B6 65.5(5) . .
C2 C1 Si1 126.7(5) . .
B5 C1 Si1 121.0(5) . .
B6 C1 Si1 124.5(5) . .
C2 C1 Tb 72.8(4) . 3_657
B5 C1 Tb 73.4(4) . 3_657
B6 C1 Tb 101.9(4) . 3_657
Si1 C1 Tb 133.5(3) . 3_657
C1 C2 B3 111.5(6) . .
C1 C2 B6 63.2(5) . .
B3 C2 B6 66.2(5) . .
C1 C2 Si2 130.7(5) . .
B3 C2 Si2 115.7(5) . .
B6 C2 Si2 125.9(5) . .
C1 C2 Tb 74.9(4) . 3_657
B3 C2 Tb 74.3(4) . 3_657
B6 C2 Tb 102.4(4) . 3_657
Si2 C2 Tb 131.1(3) . 3_657
C2 B3 B4 106.6(6) . .
C2 B3 B6 61.6(4) . .
B4 B3 B6 62.5(5) . .
C2 B3 Tb 171.0(5) . .
B4 B3 Tb 71.8(4) . .
B6 B3 Tb 123.0(4) . .
C2 B3 Tb 72.5(4) . 3_657
B4 B3 Tb 74.1(4) . 3_657
B6 B3 Tb 99.6(4) . 3_657
Tb B3 Tb 98.7(2) . 3_657
B5 B4 B3 104.1(6) . .
B5 B4 B6 61.5(5) . .
B3 B4 B6 62.5(4) . .
B5 B4 Tb 168.4(5) . .
B3 B4 Tb 72.6(4) . .
B6 B4 Tb 123.6(4) . .
B5 B4 Tb 70.8(4) . 3_657
B3 B4 Tb 70.7(4) . 3_657
B6 B4 Tb 97.8(4) . 3_657
Tb B4 Tb 97.7(2) . 3_657
C1 B5 B4 107.4(6) . .
C1 B5 B6 61.4(5) . .
B4 B5 B6 63.2(5) . .
C1 B5 Tb 73.6(4) . 3_657
B4 B5 Tb 74.1(4) . 3_657
B6 B5 Tb 100.3(4) . 3_657
C1 B6 C2 52.1(4) . .
C1 B6 B5 53.0(4) . .
C2 B6 B5 91.9(5) . .
C1 B6 B3 92.4(5) . .
C2 B6 B3 52.2(4) . .
B5 B6 B3 94.4(5) . .
C1 B6 B4 95.1(5) . .
C2 B6 B4 93.9(5) . .
B5 B6 B4 55.3(4) . .
B3 B6 B4 55.1(4) . .
C15 O11 C12 108.8(5) . .
C15 O11 Tb 126.9(4) . .
C12 O11 Tb 123.1(4) . .
O11 C12 C13 105.7(6) . .
C12 C13 C14 103.9(7) . .
C15 C14 C13 102.5(7) . .
O11 C15 C14 105.9(6) . .
C25 O21 C22 109.2(5) . .
C25 O21 Tb 121.5(4) . .
C22 O21 Tb 128.1(4) . .
O21 C22 C23 103.9(6) . .
C24 C23 C22 102.2(6) . .
C25 C24 C23 104.0(6) . .
O21 C25 C24 106.0(6) . .
C32 O31 C35 110.9(13) . .
O31 C32 C33 110.5(16) . .
C34 C33 C32 104.5(15) . .
C33 C34 C35 105.5(15) . .
O31 C35 C34 104.6(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb O21 2.383(4) .
Tb O11 2.483(5) .
Tb Cl 2.5882(19) .
Tb C2 2.702(7) 3_657
Tb B4 2.715(8) .
Tb B3 2.726(8) .
Tb B3 2.727(7) 3_657
Tb B5 2.728(8) 3_657
Tb C1 2.731(7) 3_657
Tb B4 2.778(8) 3_657
Si1 C101 1.854(10) .
Si1 C103 1.872(9) .
Si1 C102 1.874(10) .
Si1 C1 1.877(7) .
Si2 C201 1.871(9) .
Si2 C203 1.873(10) .
Si2 C202 1.875(9) .
Si2 C2 1.888(7) .
C1 C2 1.511(9) .
C1 B5 1.554(10) .
C1 B6 1.708(11) .
C1 Tb 2.731(7) 3_657
C2 B3 1.552(10) .
C2 B6 1.730(10) .
C2 Tb 2.702(7) 3_657
B3 B4 1.663(10) .
B3 B6 1.798(11) .
B3 Tb 2.727(7) 3_657
B4 B5 1.657(11) .
B4 B6 1.798(11) .
B4 Tb 2.778(8) 3_657
B5 B6 1.770(11) .
B5 Tb 2.728(8) 3_657
O11 C15 1.459(8) .
O11 C12 1.467(9) .
C12 C13 1.507(11) .
C13 C14 1.517(12) .
C14 C15 1.495(11) .
O21 C25 1.456(9) .
O21 C22 1.462(8) .
C22 C23 1.514(10) .
C23 C24 1.505(12) .
C24 C25 1.495(11) .
O31 C32 1.258(19) .
O31 C35 1.45(2) .
C32 C33 1.49(2) .
C33 C34 1.417(19) .
C34 C35 1.465(18) .
