#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075404.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_4075404
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 Br O3 Si2 Sm'
_chemical_formula_weight         664.25
_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                 108.869(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.848(3)
_cell_length_b                   11.644(2)
_cell_length_c                   16.909(3)
_cell_measurement_reflns_used    566
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2952.6(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      213(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11657
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.441
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.691728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.979
_refine_diff_density_min         -2.541
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.00000(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.539
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.539
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0955
_refine_ls_shift/su_max          1.827
_refine_ls_shift/su_mean         0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+98.5105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.1909
_reflns_number_gt                3061
_reflns_number_total             3116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060268ksi20060525_065827.cif
_cod_data_source_block           C8_hos228a
_cod_original_cell_volume        2952.7(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075404
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
Sm Sm 0.41884(6) 0.13964(8) 0.94597(6) 0.0196(4) Uani 1 1 d .
Br Br 0.38430(17) 0.34676(19) 1.00873(15) 0.0488(7) Uani 1 1 d .
Si1 Si 0.8325(4) -0.0963(6) 1.0173(4) 0.0419(17) Uani 1 1 d .
Si2 Si 0.6260(4) -0.1278(6) 0.8214(4) 0.0383(16) Uani 1 1 d .
C1 C 0.7151(13) -0.0508(18) 1.0040(11) 0.029(5) Uani 1 1 d .
C2 C 0.6377(12) -0.0626(17) 0.9268(12) 0.025(5) Uani 1 1 d .
B3 B 0.5612(14) 0.0204(17) 0.9312(12) 0.013(5) Uani 1 1 d .
H3 H 0.5121 0.0156 0.8673 0.03(5) Uiso 1 1 calc R
B4 B 0.5965(15) 0.0936(17) 1.0146(13) 0.021(6) Uani 1 1 d .
H4 H 0.5915 0.1732 1.0489 0.05(6) Uiso 1 1 calc R
B5 B 0.6971(15) 0.0385(18) 1.0625(13) 0.022(6) Uani 1 1 d .
H5 H 0.7451 0.0702 1.1219 0.01(4) Uiso 1 1 calc R
B6 B 0.6712(17) 0.074(2) 0.9572(13) 0.031(6) Uani 1 1 d .
H6 H 0.7000 0.1412 0.9269 0.03(5) Uiso 1 1 calc R
O11 O 0.4798(9) 0.2754(11) 0.8635(7) 0.028(3) Uani 1 1 d .
C12 C 0.5388(16) 0.369(2) 0.8991(13) 0.049(7) Uani 1 1 d .
H12A H 0.5908 0.3417 0.9443 0.00(4) Uiso 1 1 calc R
H12B H 0.5080 0.4270 0.9219 0.03(6) Uiso 1 1 calc R
C13 C 0.5670(16) 0.420(2) 0.8304(13) 0.045(6) Uani 1 1 d .
H13A H 0.6279 0.4499 0.8519 0.07(8) Uiso 1 1 calc R
H13B H 0.5267 0.4817 0.8020 0.00(4) Uiso 1 1 calc R
C14 C 0.5617(16) 0.321(2) 0.7729(13) 0.042(6) Uani 1 1 d .
H14A H 0.5531 0.3461 0.7156 0.08(8) Uiso 1 1 calc R
H14B H 0.6150 0.2720 0.7921 0.07(8) Uiso 1 1 calc R
C15 C 0.4812(15) 0.2601(18) 0.7795(12) 0.034(6) Uani 1 1 d .
H15A H 0.4271 0.2924 0.7395 0.01(4) Uiso 1 1 calc R
H15B H 0.4840 0.1782 0.7673 0.00(4) Uiso 1 1 calc R
O21 O 0.3189(8) 0.1304(12) 0.8042(8) 0.032(3) Uani 1 1 d .
C22 C 0.3069(12) 0.0365(17) 0.7455(12) 0.026(5) Uani 1 1 d .
H22A H 0.3210 -0.0371 0.7750 0.00(4) Uiso 1 1 calc R
H22B H 0.3451 0.0463 0.7106 0.06(8) Uiso 1 1 calc R
C23 C 0.2122(14) 0.0416(19) 0.6946(15) 0.041(6) Uani 1 1 d .
H23A H 0.1748 0.0011 0.7217 0.12(13) Uiso 1 1 calc R
H23B H 0.2023 0.0089 0.6389 0.06(7) Uiso 1 1 calc R
C24 C 0.1943(16) 0.166(2) 0.6900(18) 0.059(8) Uani 1 1 d .
H24A H 0.2101 0.2010 0.6438 0.08(10) Uiso 1 1 calc R
H24B H 0.1311 0.1814 0.6813 0.07(8) Uiso 1 1 calc R
C25 C 0.2485(14) 0.213(2) 0.7683(14) 0.044(6) Uani 1 1 d .
H25A H 0.2129 0.2242 0.8055 0.00(4) Uiso 1 1 calc R
H25B H 0.2737 0.2867 0.7599 0.11(12) Uiso 1 1 calc R
O31 O 0.889(3) 0.359(3) 1.0932(16) 0.152(13) Uani 1 1 d .
C32 C 0.936(5) 0.322(7) 1.054(3) 0.25(4) Uani 1 1 d .
H32A H 0.9488 0.2413 1.0687 0.16(17) Uiso 1 1 calc R
H32B H 0.9932 0.3637 1.0729 0.2(3) Uiso 1 1 calc R
C33 C 0.900(4) 0.332(7) 0.965(2) 0.16(2) Uani 1 1 d .
H33A H 0.9413 0.3703 0.9417 0.3(4) Uiso 1 1 calc R
H33B H 0.8838 0.2566 0.9388 0.4(6) Uiso 1 1 calc R
C34 C 0.830(3) 0.394(5) 0.958(2) 0.17(3) Uani 1 1 d .
H34A H 0.7750 0.3538 0.9265 0.11(12) Uiso 1 1 calc R
H34B H 0.8329 0.4677 0.9306 0.13(16) Uiso 1 1 calc R
C35 C 0.838(6) 0.407(7) 1.037(3) 0.48(10) Uani 1 1 d .
H35A H 0.8474 0.4889 1.0485 0.3(3) Uiso 1 1 calc R
H35B H 0.7787 0.3892 1.0409 0.01(4) Uiso 1 1 calc R
C101 C 0.849(2) -0.255(2) 1.0252(19) 0.065(8) Uani 1 1 d .
H10A H 0.8093 -0.2909 0.9752 0.3(3) Uiso 1 1 calc R
H10B H 0.8348 -0.2829 1.0736 0.06(7) Uiso 1 1 calc R
H10C H 0.9100 -0.2730 1.0310 0.15(15) Uiso 1 1 calc R
C102 C 0.8723(17) -0.039(3) 0.9334(16) 0.069(9) Uani 1 1 d .
H10D H 0.8645 0.0440 0.9301 0.09(12) Uiso 1 1 calc R
H10E H 0.8383 -0.0730 0.8804 0.02(5) Uiso 1 1 calc R
H10F H 0.9350 -0.0570 0.9458 0.05(7) Uiso 1 1 calc R
C103 C 0.9073(17) -0.037(3) 1.1171(16) 0.064(8) Uani 1 1 d .
H10G H 0.9042 0.0461 1.1154 0.00(4) Uiso 1 1 calc R
H10H H 0.9681 -0.0614 1.1252 0.02(5) Uiso 1 1 calc R
H10I H 0.8888 -0.0651 1.1630 0.2(2) Uiso 1 1 calc R
C201 C 0.7011(17) -0.249(2) 0.8160(15) 0.056(7) Uani 1 1 d .
H20A H 0.6955 -0.3100 0.8528 0.02(5) Uiso 1 1 calc R
H20B H 0.7623 -0.2218 0.8334 0.06(8) Uiso 1 1 calc R
H20C H 0.6845 -0.2771 0.7591 0.10(10) Uiso 1 1 calc R
C202 C 0.5118(18) -0.185(2) 0.7773(16) 0.060(8) Uani 1 1 d .
H20D H 0.5029 -0.2456 0.8133 0.07(9) Uiso 1 1 calc R
H20E H 0.5035 -0.2160 0.7220 0.13(14) Uiso 1 1 calc R
H20F H 0.4691 -0.1240 0.7735 0.2(2) Uiso 1 1 calc R
C203 C 0.642(2) -0.009(2) 0.7524(14) 0.062(8) Uani 1 1 d .
H20G H 0.7011 0.0227 0.7762 0.15(18) Uiso 1 1 calc R
H20H H 0.5977 0.0500 0.7482 0.09(10) Uiso 1 1 calc R
H20I H 0.6347 -0.0398 0.6973 0.05(6) 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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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 Sm O11 73.8(4) . .
O21 Sm B4 132.0(5) . .
O11 Sm B4 80.2(6) . .
O21 Sm B3 100.5(5) . .
O11 Sm B3 77.9(5) . .
B4 Sm B3 33.8(6) . .
O21 Sm C1 88.0(5) . 3_657
O11 Sm C1 153.1(5) . 3_657
B4 Sm C1 126.3(6) . 3_657
B3 Sm C1 125.8(6) . 3_657
O21 Sm B3 127.1(6) . 3_657
O11 Sm B3 152.2(5) . 3_657
B4 Sm B3 72.1(7) . 3_657
B3 Sm B3 80.0(6) . 3_657
C1 Sm B3 54.3(6) 3_657 3_657
O21 Sm C2 119.4(5) . 3_657
O11 Sm C2 158.4(5) . 3_657
B4 Sm C2 99.0(6) . 3_657
B3 Sm C2 113.3(6) . 3_657
C1 Sm C2 31.4(6) 3_657 3_657
B3 Sm C2 33.4(6) 3_657 3_657
O21 Sm B5 72.6(6) . 3_657
O11 Sm B5 145.3(5) . 3_657
B4 Sm B5 117.1(7) . 3_657
B3 Sm B5 99.8(6) . 3_657
C1 Sm B5 32.3(6) 3_657 3_657
B3 Sm B5 55.6(7) 3_657 3_657
C2 Sm B5 53.8(6) 3_657 3_657
O21 Sm Br 105.8(3) . .
O11 Sm Br 79.8(3) . .
B4 Sm Br 108.3(4) . .
B3 Sm Br 138.8(4) . .
C1 Sm Br 86.6(4) 3_657 .
B3 Sm Br 107.0(4) 3_657 .
C2 Sm Br 80.1(4) 3_657 .
B5 Sm Br 117.9(4) 3_657 .
O21 Sm B4 96.5(6) . 3_657
O11 Sm B4 144.9(5) . 3_657
B4 Sm B4 82.3(7) . 3_657
B3 Sm B4 70.7(6) . 3_657
C1 Sm B4 55.1(6) 3_657 3_657
B3 Sm B4 33.1(6) 3_657 3_657
C2 Sm B4 54.9(6) 3_657 3_657
B5 Sm B4 34.8(7) 3_657 3_657
Br Sm B4 134.9(4) . 3_657
C102 Si1 C103 106.7(13) . .
C102 Si1 C101 109.9(14) . .
C103 Si1 C101 105.7(14) . .
C102 Si1 C1 112.0(11) . .
C103 Si1 C1 108.8(11) . .
C101 Si1 C1 113.3(12) . .
C202 Si2 C201 105.4(13) . .
C202 Si2 C203 109.0(14) . .
C201 Si2 C203 108.0(13) . .
C202 Si2 C2 108.1(10) . .
C201 Si2 C2 118.6(10) . .
C203 Si2 C2 107.4(10) . .
C2 C1 B5 111.1(17) . .
C2 C1 B6 64.6(13) . .
B5 C1 B6 65.3(14) . .
C2 C1 Si1 125.9(14) . .
B5 C1 Si1 120.0(15) . .
B6 C1 Si1 122.7(14) . .
C2 C1 Sm 74.5(10) . 3_657
B5 C1 Sm 74.3(11) . 3_657
B6 C1 Sm 103.2(12) . 3_657
Si1 C1 Sm 134.1(10) . 3_657
C1 C2 B3 109.5(16) . .
C1 C2 B6 63.8(14) . .
B3 C2 B6 65.2(14) . .
C1 C2 Si2 132.0(14) . .
B3 C2 Si2 116.7(13) . .
B6 C2 Si2 125.8(13) . .
C1 C2 Sm 74.1(10) . 3_657
B3 C2 Sm 73.2(10) . 3_657
B6 C2 Sm 102.6(12) . 3_657
Si2 C2 Sm 130.8(9) . 3_657
C2 B3 B4 108.5(16) . .
C2 B3 B6 61.0(13) . .
B4 B3 B6 63.5(13) . .
C2 B3 Sm 172.3(13) . .
B4 B3 Sm 73.1(10) . .
B6 B3 Sm 125.1(12) . .
C2 B3 Sm 73.4(10) . 3_657
B4 B3 Sm 76.7(11) . 3_657
B6 B3 Sm 100.9(11) . 3_657
Sm B3 Sm 100.0(6) . 3_657
B3 B4 B5 103.4(14) . .
B3 B4 B6 63.3(12) . .
B5 B4 B6 60.8(12) . .
B3 B4 Sm 73.1(11) . .
B5 B4 Sm 167.4(14) . .
B6 B4 Sm 125.0(13) . .
B3 B4 Sm 70.2(10) . 3_657
B5 B4 Sm 69.9(10) . 3_657
B6 B4 Sm 97.5(10) . 3_657
Sm B4 Sm 97.7(7) . 3_657
C1 B5 B4 107.3(15) . .
C1 B5 B6 62.0(13) . .
B4 B5 B6 62.6(14) . .
C1 B5 Sm 73.4(11) . 3_657
B4 B5 Sm 75.3(11) . 3_657
B6 B5 Sm 101.2(12) . 3_657
C1 B6 C2 51.6(11) . .
C1 B6 B5 52.6(12) . .
C2 B6 B5 91.8(14) . .
C1 B6 B3 92.0(14) . .
C2 B6 B3 53.8(11) . .
B5 B6 B3 93.2(15) . .
C1 B6 B4 95.8(15) . .
C2 B6 B4 94.9(15) . .
B5 B6 B4 56.6(13) . .
B3 B6 B4 53.2(12) . .
C12 O11 C15 107.0(14) . .
C12 O11 Sm 124.3(11) . .
C15 O11 Sm 127.2(10) . .
O11 C12 C13 107.0(17) . .
C12 C13 C14 103.5(18) . .
C15 C14 C13 100.7(18) . .
O11 C15 C14 107.6(16) . .
C25 O21 C22 107.5(14) . .
C25 O21 Sm 123.9(11) . .
C22 O21 Sm 127.9(10) . .
O21 C22 C23 104.7(16) . .
C22 C23 C24 102.3(18) . .
C25 C24 C23 106(2) . .
C24 C25 O21 106.9(18) . .
C32 O31 C35 97(4) . .
O31 C32 C33 116(5) . .
O31 C32 C35 41(2) . .
C33 C32 C35 76(4) . .
C34 C33 C32 101(4) . .
C34 C33 C35 41(3) . .
C32 C33 C35 60(3) . .
C33 C34 C35 100(4) . .
O31 C35 C34 126(6) . .
O31 C35 C32 43(3) . .
C34 C35 C32 84(3) . .
O31 C35 C33 86(4) . .
C34 C35 C33 40(2) . .
C32 C35 C33 44(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm O21 2.410(12) .
Sm O11 2.500(12) .
Sm B4 2.73(2) .
Sm B3 2.73(2) .
Sm C1 2.730(19) 3_657
Sm B3 2.732(19) 3_657
Sm C2 2.735(18) 3_657
Sm B5 2.74(2) 3_657
Sm Br 2.760(2) .
Sm B4 2.83(2) 3_657
Si1 C102 1.85(3) .
Si1 C103 1.85(2) .
Si1 C101 1.86(3) .
Si1 C1 1.88(2) .
Si2 C202 1.84(3) .
Si2 C201 1.86(2) .
Si2 C203 1.87(2) .
Si2 C2 1.89(2) .
C1 C2 1.48(3) .
C1 B5 1.52(3) .
C1 B6 1.69(3) .
C1 Sm 2.730(19) 3_657
C2 B3 1.57(3) .
C2 B6 1.71(3) .
C2 Sm 2.735(18) 3_657
B3 B4 1.59(3) .
B3 B6 1.77(3) .
B3 Sm 2.732(19) 3_657
B4 B5 1.67(3) .
B4 B6 1.77(3) .
B4 Sm 2.83(2) 3_657
B5 B6 1.74(3) .
B5 Sm 2.74(2) 3_657
O11 C12 1.44(2) .
O11 C15 1.44(2) .
C12 C13 1.49(3) .
C13 C14 1.50(3) .
C14 C15 1.49(3) .
O21 C25 1.45(2) .
O21 C22 1.45(2) .
C22 C23 1.47(3) .
C23 C24 1.48(3) .
C24 C25 1.43(3) .
O31 C32 1.22(5) .
O31 C35 1.18(7) .
C32 C33 1.43(6) .
C32 C35 1.79(8) .
C33 C34 1.29(5) .
C33 C35 1.99(7) .
C34 C35 1.31(5) .
