#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075412.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_4075412
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 Lu O3 Si2'
_chemical_formula_weight         644.41
_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                 108.938(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.958(5)
_cell_length_b                   11.349(4)
_cell_length_c                   16.962(6)
_cell_measurement_reflns_used    701
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2905.7(17)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0214
_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            18578
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_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    3.590
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.471417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.512
_refine_diff_density_min         -1.422
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00000(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.516
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.516
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          2.411
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+15.2593P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                4983
_reflns_number_total             5043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060268ksi20060525_065827.cif
_cod_data_source_block           C16_hos222
_cod_original_cell_volume        2905.6(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075412
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
Lu Lu 0.420400(17) 0.13503(2) 0.946763(16) 0.02286(10) Uani 1 1 d .
Cl Cl 0.37923(13) 0.33014(15) 0.99594(12) 0.0408(4) Uani 1 1 d .
Si1 Si 0.82929(13) -0.0967(2) 1.01909(13) 0.0399(5) Uani 1 1 d .
Si2 Si 0.62319(13) -0.1372(2) 0.82465(12) 0.0372(4) Uani 1 1 d .
C1 C 0.7122(4) -0.0504(6) 1.0047(4) 0.0274(14) Uani 1 1 d .
C2 C 0.6336(4) -0.0656(5) 0.9277(4) 0.0249(13) Uani 1 1 d .
B3 B 0.5566(5) 0.0183(6) 0.9291(4) 0.0236(15) Uani 1 1 d .
H3 H 0.5090 0.0120 0.8649 0.06(2) Uiso 1 1 calc R
B4 B 0.5921(5) 0.0945(6) 1.0166(4) 0.0239(15) Uani 1 1 d .
H4 H 0.5865 0.1744 1.0524 0.09(3) Uiso 1 1 calc R
B5 B 0.6924(5) 0.0425(7) 1.0642(5) 0.0267(16) Uani 1 1 d .
H5 H 0.7397 0.0763 1.1234 0.024(16) Uiso 1 1 calc R
B6 B 0.6661(5) 0.0768(7) 0.9565(5) 0.0286(16) Uani 1 1 d .
H6 H 0.6936 0.1457 0.9254 0.032(18) Uiso 1 1 calc R
O11 O 0.4812(3) 0.2744(4) 0.8700(3) 0.0323(10) Uani 1 1 d .
C12 C 0.5360(6) 0.3748(7) 0.9090(5) 0.052(2) Uani 1 1 d .
H12A H 0.5880 0.3486 0.9547 0.08(3) Uiso 1 1 calc R
H12B H 0.5022 0.4301 0.9313 0.07(3) Uiso 1 1 calc R
C13 C 0.5638(6) 0.4323(7) 0.8415(5) 0.051(2) Uani 1 1 d .
H13A H 0.6234 0.4658 0.8641 0.07(3) Uiso 1 1 calc R
H13B H 0.5223 0.4948 0.8138 0.06(3) Uiso 1 1 calc R
C14 C 0.5618(6) 0.3320(7) 0.7820(5) 0.049(2) Uani 1 1 d .
H14A H 0.5529 0.3611 0.7255 0.06(2) Uiso 1 1 calc R
H14B H 0.6165 0.2856 0.8008 0.07(3) Uiso 1 1 calc R
C15 C 0.4840(5) 0.2617(7) 0.7858(4) 0.0397(17) Uani 1 1 d .
H15A H 0.4292 0.2916 0.7454 0.08(3) Uiso 1 1 calc R
H15B H 0.4909 0.1787 0.7734 0.032(19) Uiso 1 1 calc R
O21 O 0.3281(3) 0.1281(4) 0.8108(3) 0.0294(10) Uani 1 1 d .
C22 C 0.3152(4) 0.0313(6) 0.7506(4) 0.0296(15) Uani 1 1 d .
H22A H 0.3265 -0.0451 0.7791 0.030(18) Uiso 1 1 calc R
H22B H 0.3545 0.0400 0.7170 0.026(17) Uiso 1 1 calc R
C23 C 0.2194(5) 0.0423(7) 0.6972(5) 0.0401(18) Uani 1 1 d .
H23A H 0.2095 0.0089 0.6416 0.04(2) Uiso 1 1 calc R
H23B H 0.1803 0.0031 0.7232 0.05(2) Uiso 1 1 calc R
C24 C 0.2050(6) 0.1734(7) 0.6930(5) 0.049(2) Uani 1 1 d .
H24A H 0.2271 0.2091 0.6509 0.05(3) Uiso 1 1 calc R
H24B H 0.1421 0.1924 0.6797 0.10(4) Uiso 1 1 calc R
C25 C 0.2570(5) 0.2150(7) 0.7783(5) 0.0442(19) Uani 1 1 d .
H25A H 0.2818 0.2934 0.7759 0.06(3) Uiso 1 1 calc R
H25B H 0.2193 0.2188 0.8138 0.04(2) Uiso 1 1 calc R
O31 O 0.8861(8) 0.3671(13) 1.0915(5) 0.147(5) Uani 1 1 d .
C32 C 0.9485(13) 0.338(2) 1.0621(9) 0.146(8) Uani 1 1 d .
H32A H 0.9723 0.2604 1.0840 0.24(11) Uiso 1 1 calc R
H32B H 0.9967 0.3953 1.0797 0.4(2) Uiso 1 1 calc R
C33 C 0.9126(11) 0.333(2) 0.9696(9) 0.136(7) Uani 1 1 d .
H33A H 0.9507 0.3772 0.9448 0.25(12) Uiso 1 1 calc R
H33B H 0.9079 0.2516 0.9498 0.4(2) Uiso 1 1 calc R
C34 C 0.8272(8) 0.3864(18) 0.9489(8) 0.104(5) Uani 1 1 d .
H34A H 0.7840 0.3424 0.9042 0.17(7) Uiso 1 1 calc R
H34B H 0.8292 0.4678 0.9303 0.19(9) Uiso 1 1 calc R
C35 C 0.8024(11) 0.384(2) 1.0257(8) 0.124(6) Uani 1 1 d .
H35A H 0.7743 0.4578 1.0330 0.35(18) Uiso 1 1 calc R
H35B H 0.7618 0.3183 1.0242 1.5(12) Uiso 1 1 calc R
C101 C 0.8476(6) -0.2596(8) 1.0320(6) 0.058(2) Uani 1 1 d .
H10A H 0.8093 -0.2998 0.9831 0.09(4) Uiso 1 1 calc R
H10B H 0.8339 -0.2858 1.0809 0.13(5) Uiso 1 1 calc R
H10C H 0.9089 -0.2775 1.0387 0.12(4) Uiso 1 1 calc R
C102 C 0.8669(5) -0.0415(10) 0.9321(5) 0.058(2) Uani 1 1 d .
H10D H 0.8595 0.0434 0.9276 0.06(3) Uiso 1 1 calc R
H10E H 0.8318 -0.0781 0.8802 0.07(3) Uiso 1 1 calc R
H10F H 0.9289 -0.0611 0.9435 0.12(5) Uiso 1 1 calc R
C103 C 0.9050(5) -0.0276(9) 1.1167(5) 0.055(2) Uani 1 1 d .
H10G H 0.8997 0.0575 1.1123 0.05(3) Uiso 1 1 calc R
H10H H 0.9657 -0.0504 1.1242 0.08(3) Uiso 1 1 calc R
H10I H 0.8887 -0.0541 1.1641 0.07(3) Uiso 1 1 calc R
C201 C 0.6998(6) -0.2610(8) 0.8237(6) 0.054(2) Uani 1 1 d .
H20A H 0.6937 -0.3227 0.8610 0.08(3) Uiso 1 1 calc R
H20B H 0.7604 -0.2324 0.8419 0.09(3) Uiso 1 1 calc R
H20C H 0.6851 -0.2922 0.7676 0.10(4) Uiso 1 1 calc R
C202 C 0.5090(5) -0.2013(9) 0.7830(6) 0.058(3) Uani 1 1 d .
H20D H 0.5019 -0.2620 0.8207 0.10(4) Uiso 1 1 calc R
H20E H 0.5004 -0.2355 0.7285 0.07(3) Uiso 1 1 calc R
H20F H 0.4655 -0.1397 0.7783 0.08(3) Uiso 1 1 calc R
C203 C 0.6349(8) -0.0193(10) 0.7516(6) 0.069(3) Uani 1 1 d .
H20G H 0.6935 0.0154 0.7730 0.10(4) Uiso 1 1 calc R
H20H H 0.5905 0.0411 0.7469 0.14(6) Uiso 1 1 calc R
H20I H 0.6267 -0.0534 0.6972 0.12(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'
Lu Lu -0.4720 5.8584 '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 Lu O11 73.94(15) . .
O21 Lu Cl 102.14(12) . .
O11 Lu Cl 78.43(12) . .
O21 Lu B3 98.74(19) . .
O11 Lu B3 77.33(19) . .
Cl Lu B3 141.98(16) . .
O21 Lu B4 132.51(18) . .
O11 Lu B4 79.55(19) . .
Cl Lu B4 110.28(16) . .
B3 Lu B4 36.4(2) . .
O21 Lu C2 121.58(18) . 3_657
O11 Lu C2 154.98(17) . 3_657
Cl Lu C2 78.98(14) . 3_657
B3 Lu C2 115.7(2) . 3_657
B4 Lu C2 98.4(2) . 3_657
O21 Lu B3 130.51(19) . 3_657
O11 Lu B3 150.25(19) . 3_657
Cl Lu B3 107.19(16) . 3_657
B3 Lu B3 81.6(2) . 3_657
B4 Lu B3 71.1(2) . 3_657
C2 Lu B3 34.1(2) 3_657 3_657
O21 Lu B5 72.91(19) . 3_657
O11 Lu B5 145.91(19) . 3_657
Cl Lu B5 116.29(17) . 3_657
B3 Lu B5 100.0(2) . 3_657
B4 Lu B5 118.5(2) . 3_657
C2 Lu B5 56.4(2) 3_657 3_657
B3 Lu B5 58.6(2) 3_657 3_657
O21 Lu C1 89.05(18) . 3_657
O11 Lu C1 152.22(18) . 3_657
Cl Lu C1 84.08(15) . 3_657
B3 Lu C1 127.9(2) . 3_657
B4 Lu C1 127.2(2) . 3_657
C2 Lu C1 32.54(19) 3_657 3_657
B3 Lu C1 56.2(2) 3_657 3_657
B5 Lu C1 33.9(2) 3_657 3_657
O21 Lu B4 97.28(18) . 3_657
O11 Lu B4 145.02(18) . 3_657
Cl Lu B4 136.30(15) . 3_657
B3 Lu B4 70.6(2) . 3_657
B4 Lu B4 82.7(2) . 3_657
C2 Lu B4 57.6(2) 3_657 3_657
B3 Lu B4 35.9(2) 3_657 3_657
B5 Lu B4 35.8(2) 3_657 3_657
C1 Lu B4 57.3(2) 3_657 3_657
C102 Si1 C101 110.2(5) . .
C102 Si1 C103 106.0(4) . .
C101 Si1 C103 106.2(4) . .
C102 Si1 C1 111.3(4) . .
C101 Si1 C1 113.7(4) . .
C103 Si1 C1 109.0(4) . .
C201 Si2 C203 109.0(5) . .
C201 Si2 C202 105.3(4) . .
C203 Si2 C202 108.8(5) . .
C201 Si2 C2 118.2(3) . .
C203 Si2 C2 107.9(4) . .
C202 Si2 C2 107.4(3) . .
C2 C1 B5 110.7(5) . .
C2 C1 B6 64.6(4) . .
B5 C1 B6 65.9(4) . .
C2 C1 Si1 126.7(5) . .
B5 C1 Si1 120.4(5) . .
B6 C1 Si1 123.8(4) . .
C2 C1 Lu 72.9(3) . 3_657
B5 C1 Lu 72.4(3) . 3_657
B6 C1 Lu 100.9(4) . 3_657
Si1 C1 Lu 135.2(3) . 3_657
C1 C2 B3 110.9(5) . .
C1 C2 B6 63.5(4) . .
B3 C2 B6 65.7(4) . .
C1 C2 Si2 130.9(5) . .
B3 C2 Si2 116.4(4) . .
B6 C2 Si2 126.6(4) . .
C1 C2 Lu 74.6(3) . 3_657
B3 C2 Lu 73.0(3) . 3_657
B6 C2 Lu 101.4(4) . 3_657
Si2 C2 Lu 131.3(3) . 3_657
C2 B3 B4 107.0(5) . .
C2 B3 B6 61.4(4) . .
B4 B3 B6 63.3(4) . .
C2 B3 Lu 171.0(5) . .
B4 B3 Lu 72.0(3) . .
B6 B3 Lu 123.8(4) . .
C2 B3 Lu 72.9(3) . 3_657
B4 B3 Lu 73.3(3) . 3_657
B6 B3 Lu 99.5(4) . 3_657
Lu B3 Lu 98.4(2) . 3_657
B5 B4 B3 104.3(5) . .
B5 B4 B6 61.8(4) . .
B3 B4 B6 62.0(4) . .
B5 B4 Lu 168.3(5) . .
B3 B4 Lu 71.7(3) . .
B6 B4 Lu 122.6(4) . .
B5 B4 Lu 71.0(4) . 3_657
B3 B4 Lu 70.9(3) . 3_657
B6 B4 Lu 97.7(4) . 3_657
Lu B4 Lu 97.3(2) . 3_657
C1 B5 B4 107.0(5) . .
C1 B5 B6 60.9(4) . .
B4 B5 B6 63.4(4) . .
C1 B5 Lu 73.7(4) . 3_657
B4 B5 Lu 73.2(4) . 3_657
B6 B5 Lu 99.5(4) . 3_657
C1 B6 C2 51.9(4) . .
C1 B6 B5 53.2(4) . .
C2 B6 B5 92.0(5) . .
C1 B6 B3 92.5(5) . .
C2 B6 B3 52.9(4) . .
B5 B6 B3 94.0(5) . .
C1 B6 B4 94.8(5) . .
C2 B6 B4 94.1(5) . .
B5 B6 B4 54.8(4) . .
B3 B6 B4 54.7(4) . .
C15 O11 C12 108.6(5) . .
C15 O11 Lu 127.2(4) . .
C12 O11 Lu 123.2(4) . .
O11 C12 C13 106.0(6) . .
C12 C13 C14 103.5(6) . .
C15 C14 C13 102.2(6) . .
O11 C15 C14 106.3(6) . .
C22 O21 C25 108.9(5) . .
C22 O21 Lu 128.5(4) . .
C25 O21 Lu 121.3(4) . .
O21 C22 C23 104.0(5) . .
C24 C23 C22 102.7(6) . .
C25 C24 C23 103.8(6) . .
O21 C25 C24 105.7(6) . .
C32 O31 C35 111.6(11) . .
O31 C32 C33 109.6(14) . .
C34 C33 C32 104.7(14) . .
C33 C34 C35 106.3(13) . .
O31 C35 C34 103.8(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu O21 2.299(4) .
Lu O11 2.442(4) .
Lu Cl 2.5271(18) .
Lu B3 2.644(7) .
Lu B4 2.648(7) .
Lu C2 2.662(6) 3_657
Lu B3 2.663(7) 3_657
Lu B5 2.668(7) 3_657
Lu C1 2.686(6) 3_657
Lu B4 2.700(7) 3_657
Si1 C102 1.872(9) .
Si1 C101 1.873(9) .
Si1 C103 1.876(8) .
Si1 C1 1.879(7) .
Si2 C201 1.866(8) .
Si2 C203 1.874(10) .
Si2 C202 1.875(9) .
Si2 C2 1.885(6) .
C1 C2 1.499(9) .
C1 B5 1.562(10) .
C1 B6 1.703(10) .
C1 Lu 2.686(6) 3_657
C2 B3 1.561(9) .
C2 B6 1.719(9) .
C2 Lu 2.662(6) 3_657
B3 B4 1.651(9) .
B3 B6 1.785(10) .
B3 Lu 2.663(7) 3_657
B4 B5 1.651(10) .
B4 B6 1.806(10) .
B4 Lu 2.700(7) 3_657
B5 B6 1.780(10) .
B5 Lu 2.668(7) 3_657
O11 C15 1.449(8) .
O11 C12 1.458(8) .
C12 C13 1.504(11) .
C13 C14 1.514(12) .
C14 C15 1.495(10) .
O21 C22 1.469(7) .
O21 C25 1.469(8) .
C22 C23 1.508(9) .
C23 C24 1.503(11) .
C24 C25 1.492(10) .
O31 C32 1.293(17) .
O31 C35 1.448(17) .
C32 C33 1.487(19) .
C33 C34 1.427(18) .
C34 C35 1.479(16) .
