#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075408.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_4075408
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 Ho O3 Si2'
_chemical_formula_weight         634.37
_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                 108.957(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.878(3)
_cell_length_b                   11.338(2)
_cell_length_c                   16.909(4)
_cell_measurement_reflns_used    183
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2878.9(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      213(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0262
_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            18909
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_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    2.943
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.310280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.654
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.00012(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.426
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.426
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0394P)²+25.4427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                4947
_reflns_number_total             4997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060268ksi20060525_065827.cif
_cod_data_source_block           C12_hos235
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075408
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
Ho Ho 0.41960(2) 0.13779(3) 0.94649(2) 0.02475(16) Uani 1 1 d .
Cl Cl 0.38061(18) 0.3347(2) 0.99926(16) 0.0432(6) Uani 1 1 d .
Si1 Si 0.83028(17) -0.0978(3) 1.01917(18) 0.0420(7) Uani 1 1 d .
Si2 Si 0.62443(18) -0.1347(3) 0.82418(16) 0.0390(6) Uani 1 1 d .
C1 C 0.7134(5) -0.0499(8) 1.0044(5) 0.0295(19) Uani 1 1 d .
C2 C 0.6349(5) -0.0652(8) 0.9273(5) 0.0282(18) Uani 1 1 d .
B3 B 0.5580(6) 0.0183(8) 0.9282(6) 0.0245(19) Uani 1 1 d .
H3 H 0.5101 0.0120 0.8637 0.06(3) Uiso 1 1 calc R
B4 B 0.5946(6) 0.0954(8) 1.0161(6) 0.026(2) Uani 1 1 d .
H4 H 0.5896 0.1761 1.0514 0.06(4) Uiso 1 1 calc R
B5 B 0.6941(6) 0.0428(9) 1.0638(6) 0.030(2) Uani 1 1 d .
H5 H 0.7414 0.0768 1.1232 0.03(2) Uiso 1 1 calc R
B6 B 0.6688(7) 0.0767(9) 0.9567(6) 0.030(2) Uani 1 1 d .
H6 H 0.6972 0.1454 0.9260 0.05(3) Uiso 1 1 calc R
O11 O 0.4799(4) 0.2779(5) 0.8678(4) 0.0341(14) Uani 1 1 d .
C12 C 0.5347(8) 0.3788(10) 0.9064(7) 0.052(3) Uani 1 1 d .
H12A H 0.5862 0.3533 0.9533 0.09(5) Uiso 1 1 calc R
H12B H 0.5000 0.4353 0.9271 0.04(3) Uiso 1 1 calc R
C13 C 0.5642(8) 0.4335(10) 0.8394(7) 0.052(3) Uani 1 1 d .
H13A H 0.6245 0.4660 0.8626 0.04(3) Uiso 1 1 calc R
H13B H 0.5235 0.4965 0.8107 0.05(3) Uiso 1 1 calc R
C14 C 0.5622(7) 0.3320(10) 0.7805(7) 0.050(3) Uani 1 1 d .
H14A H 0.5542 0.3601 0.7237 0.06(4) Uiso 1 1 calc R
H14B H 0.6167 0.2847 0.8001 0.05(3) Uiso 1 1 calc R
C15 C 0.4833(7) 0.2641(9) 0.7841(6) 0.042(2) Uani 1 1 d .
H15A H 0.4287 0.2948 0.7432 0.10(5) Uiso 1 1 calc R
H15B H 0.4893 0.1806 0.7719 0.011(18) Uiso 1 1 calc R
O21 O 0.3253(4) 0.1283(5) 0.8075(3) 0.0315(13) Uani 1 1 d .
C22 C 0.3134(6) 0.0314(8) 0.7485(5) 0.033(2) Uani 1 1 d .
H22A H 0.3260 -0.0445 0.7777 0.013(19) Uiso 1 1 calc R
H22B H 0.3523 0.0406 0.7143 0.06(3) Uiso 1 1 calc R
C23 C 0.2171(6) 0.0399(10) 0.6958(6) 0.045(2) Uani 1 1 d .
H23A H 0.2071 0.0054 0.6403 0.05(3) Uiso 1 1 calc R
H23B H 0.1788 0.0001 0.7226 0.05(3) Uiso 1 1 calc R
C24 C 0.2008(8) 0.1691(10) 0.6902(7) 0.054(3) Uani 1 1 d .
H24A H 0.1374 0.1865 0.6783 0.09(5) Uiso 1 1 calc R
H24B H 0.2206 0.2044 0.6464 0.10(5) Uiso 1 1 calc R
C25 C 0.2545(7) 0.2142(9) 0.7745(6) 0.047(3) Uani 1 1 d .
H25A H 0.2794 0.2920 0.7699 0.07(4) Uiso 1 1 calc R
H25B H 0.2177 0.2206 0.8109 0.05(3) Uiso 1 1 calc R
O31 O 0.8856(12) 0.3680(17) 1.0904(7) 0.149(7) Uani 1 1 d .
C32 C 0.9471(19) 0.337(4) 1.0620(13) 0.160(12) Uani 1 1 d .
H32A H 0.9693 0.2587 1.0834 0.23(15) Uiso 1 1 calc R
H32B H 0.9967 0.3930 1.0803 0.4(3) Uiso 1 1 calc R
C33 C 0.9115(17) 0.334(3) 0.9695(12) 0.133(9) Uani 1 1 d .
H33A H 0.9505 0.3780 0.9453 0.24(17) Uiso 1 1 calc R
H33B H 0.9060 0.2529 0.9489 0.3(3) Uiso 1 1 calc R
C34 C 0.8273(11) 0.388(2) 0.9488(11) 0.102(6) Uani 1 1 d .
H34A H 0.7838 0.3460 0.9030 0.18(10) Uiso 1 1 calc R
H34B H 0.8304 0.4704 0.9317 0.22(14) Uiso 1 1 calc R
C35 C 0.8025(15) 0.383(3) 1.0257(11) 0.130(9) Uani 1 1 d .
H35A H 0.7731 0.4558 1.0335 0.5(4) Uiso 1 1 calc R
H35B H 0.7628 0.3160 1.0239 1.3(18) Uiso 1 1 calc R
C101 C 0.8469(8) -0.2600(11) 1.0316(9) 0.060(3) Uani 1 1 d .
H10A H 0.8084 -0.2996 0.9823 0.06(3) Uiso 1 1 calc R
H10B H 0.8325 -0.2861 1.0804 0.13(7) Uiso 1 1 calc R
H10C H 0.9085 -0.2790 1.0388 0.11(5) Uiso 1 1 calc R
C102 C 0.8690(7) -0.0430(13) 0.9326(7) 0.061(3) Uani 1 1 d .
H10D H 0.8617 0.0419 0.9278 0.06(4) Uiso 1 1 calc R
H10E H 0.8341 -0.0798 0.8804 0.10(5) Uiso 1 1 calc R
H10F H 0.9314 -0.0628 0.9445 0.12(6) Uiso 1 1 calc R
C103 C 0.9061(7) -0.0298(12) 1.1165(7) 0.059(3) Uani 1 1 d .
H10G H 0.9010 0.0554 1.1123 0.03(3) Uiso 1 1 calc R
H10H H 0.9670 -0.0528 1.1238 0.08(4) Uiso 1 1 calc R
H10I H 0.8898 -0.0566 1.1641 0.07(4) Uiso 1 1 calc R
C201 C 0.7005(8) -0.2587(11) 0.8226(7) 0.056(3) Uani 1 1 d .
H20A H 0.6944 -0.3205 0.8600 0.07(4) Uiso 1 1 calc R
H20B H 0.7615 -0.2305 0.8407 0.11(6) Uiso 1 1 calc R
H20C H 0.6853 -0.2898 0.7662 0.11(6) Uiso 1 1 calc R
C202 C 0.5106(8) -0.1980(12) 0.7822(7) 0.063(4) Uani 1 1 d .
H20D H 0.5033 -0.2589 0.8198 0.12(7) Uiso 1 1 calc R
H20E H 0.5021 -0.2318 0.7275 0.06(3) Uiso 1 1 calc R
H20F H 0.4669 -0.1363 0.7775 0.10(6) Uiso 1 1 calc R
C203 C 0.6370(11) -0.0174(13) 0.7522(7) 0.071(4) Uani 1 1 d .
H20G H 0.6960 0.0170 0.7741 0.08(5) Uiso 1 1 calc R
H20H H 0.5925 0.0433 0.7473 0.11(6) Uiso 1 1 calc R
H20I H 0.6290 -0.0512 0.6975 0.12(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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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 Ho O11 73.8(2) . .
O21 Ho Cl 104.02(16) . .
O11 Ho Cl 78.78(16) . .
O21 Ho C2 121.2(2) . 3_657
O11 Ho C2 156.0(2) . 3_657
Cl Ho C2 79.20(19) . 3_657
O21 Ho B3 98.1(2) . .
O11 Ho B3 77.7(2) . .
Cl Ho B3 141.5(2) . .
C2 Ho B3 115.2(3) 3_657 .
O21 Ho B4 131.6(3) . .
O11 Ho B4 79.8(3) . .
Cl Ho B4 109.7(2) . .
C2 Ho B4 98.7(3) 3_657 .
B3 Ho B4 36.0(3) . .
O21 Ho B3 129.6(3) . 3_657
O11 Ho B3 151.1(2) . 3_657
Cl Ho B3 106.5(2) . 3_657
C2 Ho B3 33.5(3) 3_657 3_657
B3 Ho B3 81.7(3) . 3_657
B4 Ho B3 71.6(3) . 3_657
O21 Ho C1 89.0(2) . 3_657
O11 Ho C1 152.5(2) . 3_657
Cl Ho C1 85.0(2) . 3_657
C2 Ho C1 32.2(2) 3_657 3_657
B3 Ho C1 126.9(3) . 3_657
B4 Ho C1 126.9(3) . 3_657
B3 Ho C1 55.4(3) 3_657 3_657
O21 Ho B5 72.8(3) . 3_657
O11 Ho B5 145.7(2) . 3_657
Cl Ho B5 116.9(2) . 3_657
C2 Ho B5 55.6(3) 3_657 3_657
B3 Ho B5 99.5(3) . 3_657
B4 Ho B5 117.9(3) . 3_657
B3 Ho B5 57.8(3) 3_657 3_657
C1 Ho B5 33.4(3) 3_657 3_657
O21 Ho B4 96.5(2) . 3_657
O11 Ho B4 145.4(3) . 3_657
Cl Ho B4 135.6(2) . 3_657
C2 Ho B4 56.5(3) 3_657 3_657
B3 Ho B4 70.8(3) . 3_657
B4 Ho B4 83.0(3) . 3_657
B3 Ho B4 35.5(3) 3_657 3_657
C1 Ho B4 56.1(3) 3_657 3_657
B5 Ho B4 35.0(3) 3_657 3_657
C101 Si1 C103 106.4(6) . .
C101 Si1 C102 110.3(7) . .
C103 Si1 C102 105.8(6) . .
C101 Si1 C1 113.6(5) . .
C103 Si1 C1 109.1(5) . .
C102 Si1 C1 111.3(5) . .
C203 Si2 C202 109.0(7) . .
C203 Si2 C201 108.9(6) . .
C202 Si2 C201 105.0(6) . .
C203 Si2 C2 108.3(5) . .
C202 Si2 C2 107.4(5) . .
C201 Si2 C2 118.0(5) . .
C2 C1 B5 111.1(7) . .
C2 C1 B6 65.1(6) . .
B5 C1 B6 65.9(6) . .
C2 C1 Si1 126.4(6) . .
B5 C1 Si1 120.4(6) . .
B6 C1 Si1 123.7(6) . .
C2 C1 Ho 73.2(5) . 3_657
B5 C1 Ho 73.3(5) . 3_657
B6 C1 Ho 102.3(5) . 3_657
Si1 C1 Ho 133.9(4) . 3_657
C1 C2 B3 111.0(7) . .
C1 C2 B6 62.9(6) . .
B3 C2 B6 66.4(6) . .
C1 C2 Si2 131.2(6) . .
B3 C2 Si2 115.7(6) . .
B6 C2 Si2 126.1(6) . .
C1 C2 Ho 74.6(5) . 3_657
B3 C2 Ho 73.8(5) . 3_657
B6 C2 Ho 102.0(5) . 3_657
Si2 C2 Ho 131.2(4) . 3_657
C2 B3 B4 106.4(7) . .
C2 B3 B6 61.3(5) . .
B4 B3 B6 62.4(6) . .
C2 B3 Ho 170.8(6) . .
B4 B3 Ho 72.1(5) . .
B6 B3 Ho 123.4(6) . .
C2 B3 Ho 72.7(5) . 3_657
B4 B3 Ho 73.9(5) . 3_657
B6 B3 Ho 99.4(5) . 3_657
Ho B3 Ho 98.3(3) . 3_657
B5 B4 B3 104.5(7) . .
B5 B4 B6 61.8(6) . .
B3 B4 B6 62.5(5) . .
B5 B4 Ho 167.9(6) . .
B3 B4 Ho 71.9(4) . .
B6 B4 Ho 123.4(5) . .
B5 B4 Ho 71.0(5) . 3_657
B3 B4 Ho 70.6(5) . 3_657
B6 B4 Ho 97.6(5) . 3_657
Ho B4 Ho 97.0(3) . 3_657
C1 B5 B4 106.9(7) . .
C1 B5 B6 60.7(6) . .
B4 B5 B6 63.5(6) . .
C1 B5 Ho 73.3(5) . 3_657
B4 B5 Ho 74.1(5) . 3_657
B6 B5 Ho 100.0(5) . 3_657
C1 B6 C2 52.0(5) . .
C1 B6 B5 53.4(5) . .
C2 B6 B5 92.2(6) . .
C1 B6 B4 94.8(7) . .
C2 B6 B4 94.1(6) . .
B5 B6 B4 54.8(5) . .
C1 B6 B3 92.1(6) . .
C2 B6 B3 52.3(5) . .
B5 B6 B3 94.2(6) . .
B4 B6 B3 55.1(5) . .
C15 O11 C12 108.5(7) . .
C15 O11 Ho 127.3(5) . .
C12 O11 Ho 123.1(5) . .
O11 C12 C13 106.0(8) . .
C12 C13 C14 103.8(9) . .
C15 C14 C13 101.8(9) . .
O11 C15 C14 106.5(8) . .
C22 O21 C25 109.3(6) . .
C22 O21 Ho 128.4(5) . .
C25 O21 Ho 121.1(5) . .
O21 C22 C23 103.9(7) . .
C24 C23 C22 103.0(8) . .
C23 C24 C25 104.1(8) . .
O21 C25 C24 105.5(8) . .
C32 O31 C35 112.1(16) . .
O31 C32 C33 109(2) . .
C34 C33 C32 105.1(18) . .
C33 C34 C35 105.4(18) . .
O31 C35 C34 103.7(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho O21 2.343(5) .
Ho O11 2.457(6) .
Ho Cl 2.554(2) .
Ho C2 2.679(8) 3_657
Ho B3 2.683(9) .
Ho B4 2.686(9) .
Ho B3 2.694(9) 3_657
Ho C1 2.698(9) 3_657
Ho B5 2.698(10) 3_657
Ho B4 2.745(10) 3_657
Si1 C101 1.860(13) .
Si1 C103 1.861(11) .
Si1 C102 1.869(12) .
Si1 C1 1.871(9) .
Si2 C203 1.857(13) .
Si2 C202 1.858(12) .
Si2 C201 1.860(11) .
Si2 C2 1.871(9) .
C1 C2 1.492(11) .
C1 B5 1.552(13) .
C1 B6 1.685(13) .
C1 Ho 2.698(9) 3_657
C2 B3 1.549(13) .
C2 B6 1.718(13) .
C2 Ho 2.679(8) 3_657
B3 B4 1.659(13) .
B3 B6 1.794(13) .
B3 Ho 2.694(9) 3_657
B4 B5 1.635(13) .
B4 B6 1.791(14) .
B4 Ho 2.745(10) 3_657
B5 B6 1.764(14) .
B5 Ho 2.698(9) 3_657
O11 C15 1.441(11) .
O11 C12 1.457(11) .
C12 C13 1.494(15) .
C13 C14 1.515(16) .
C14 C15 1.490(14) .
O21 C22 1.455(10) .
O21 C25 1.455(11) .
C22 C23 1.501(12) .
C23 C24 1.486(15) .
C24 C25 1.494(14) .
O31 C32 1.27(2) .
O31 C35 1.42(2) .
C32 C33 1.48(3) .
C33 C34 1.41(2) .
C34 C35 1.48(2) .
