#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075407.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_4075407
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 Dy O3 Si2'
_chemical_formula_weight         631.94
_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                 108.928(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.951(3)
_cell_length_b                   11.403(2)
_cell_length_c                   16.982(3)
_cell_measurement_reflns_used    218
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2921.8(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      203(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0203
_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            19792
_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    2.749
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.620831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.094
_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   1.456
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.456
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          2.515
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+10.4330P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                5017
_reflns_number_total             5140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060268ksi20060525_065827.cif
_cod_data_source_block           C11_hos217
_cod_original_cell_volume        2921.9(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4075407
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
Dy Dy 0.419213(15) 0.13872(2) 0.946322(14) 0.02545(10) Uani 1 1 d .
Cl Cl 0.38098(11) 0.33600(12) 1.00026(10) 0.0447(4) Uani 1 1 d .
Si1 Si 0.83057(10) -0.09827(17) 1.01915(11) 0.0420(4) Uani 1 1 d .
Si2 Si 0.62453(11) -0.13461(16) 0.82390(10) 0.0394(4) Uani 1 1 d .
C1 C 0.7137(3) -0.0508(5) 1.0049(3) 0.0302(11) Uani 1 1 d .
C2 C 0.6352(3) -0.0655(5) 0.9272(3) 0.0285(11) Uani 1 1 d .
B3 B 0.5580(4) 0.0179(5) 0.9286(3) 0.0264(12) Uani 1 1 d .
H3 H 0.5103 0.0113 0.8645 0.06(2) Uiso 1 1 calc R
B4 B 0.5944(4) 0.0944(5) 1.0163(3) 0.0272(12) Uani 1 1 d .
H4 H 0.5892 0.1742 1.0518 0.10(3) Uiso 1 1 calc R
B5 B 0.6947(4) 0.0420(5) 1.0644(4) 0.0298(13) Uani 1 1 d .
H5 H 0.7420 0.0756 1.1235 0.019(12) Uiso 1 1 calc R
B6 B 0.6681(4) 0.0768(6) 0.9568(4) 0.0315(13) Uani 1 1 d .
H6 H 0.6957 0.1457 0.9261 0.047(17) Uiso 1 1 calc R
O11 O 0.4797(3) 0.2786(3) 0.8678(2) 0.0345(9) Uani 1 1 d .
C12 C 0.5345(5) 0.3793(6) 0.9059(4) 0.0516(17) Uani 1 1 d .
H12A H 0.5857 0.3542 0.9527 0.06(2) Uiso 1 1 calc R
H12B H 0.5001 0.4358 0.9263 0.06(2) Uiso 1 1 calc R
C13 C 0.5642(5) 0.4331(6) 0.8389(4) 0.0524(17) Uani 1 1 d .
H13A H 0.6242 0.4651 0.8619 0.06(2) Uiso 1 1 calc R
H13B H 0.5239 0.4958 0.8102 0.06(2) Uiso 1 1 calc R
C14 C 0.5618(5) 0.3315(6) 0.7805(4) 0.0500(16) Uani 1 1 d .
H14A H 0.5545 0.3591 0.7241 0.047(17) Uiso 1 1 calc R
H14B H 0.6158 0.2840 0.8005 0.07(2) Uiso 1 1 calc R
C15 C 0.4821(4) 0.2637(5) 0.7834(3) 0.0426(14) Uani 1 1 d .
H15A H 0.4280 0.2947 0.7427 0.06(2) Uiso 1 1 calc R
H15B H 0.4879 0.1806 0.7713 0.040(16) Uiso 1 1 calc R
O21 O 0.3246(2) 0.1284(3) 0.8067(2) 0.0328(8) Uani 1 1 d .
C22 C 0.3126(4) 0.0315(5) 0.7479(3) 0.0340(12) Uani 1 1 d .
H22A H 0.3260 -0.0437 0.7773 0.012(11) Uiso 1 1 calc R
H22B H 0.3511 0.0409 0.7136 0.042(17) Uiso 1 1 calc R
C23 C 0.2165(4) 0.0380(6) 0.6954(4) 0.0447(15) Uani 1 1 d .
H23A H 0.1786 -0.0015 0.7224 0.042(17) Uiso 1 1 calc R
H23B H 0.2066 0.0034 0.6403 0.056(19) Uiso 1 1 calc R
C24 C 0.2002(5) 0.1690(6) 0.6896(4) 0.0529(17) Uani 1 1 d .
H24A H 0.2203 0.2038 0.6461 0.08(3) Uiso 1 1 calc R
H24B H 0.1372 0.1866 0.6776 0.08(2) Uiso 1 1 calc R
C25 C 0.2534(4) 0.2136(5) 0.7732(4) 0.0467(16) Uani 1 1 d .
H25A H 0.2779 0.2912 0.7687 0.06(2) Uiso 1 1 calc R
H25B H 0.2166 0.2198 0.8094 0.06(2) Uiso 1 1 calc R
O31 O 0.8863(7) 0.3665(10) 1.0905(4) 0.151(4) Uani 1 1 d .
C32 C 0.9472(12) 0.337(2) 1.0616(7) 0.169(8) Uani 1 1 d .
H32A H 0.9699 0.2591 1.0828 0.28(11) Uiso 1 1 calc R
H32B H 0.9963 0.3928 1.0798 0.4(2) Uiso 1 1 calc R
C33 C 0.9124(10) 0.334(2) 0.9693(7) 0.144(6) Uani 1 1 d .
H33A H 0.9509 0.3781 0.9454 0.28(11) Uiso 1 1 calc R
H33B H 0.9078 0.2529 0.9488 0.31(13) Uiso 1 1 calc R
C34 C 0.8276(7) 0.3865(15) 0.9488(7) 0.110(4) Uani 1 1 d .
H34A H 0.7845 0.3429 0.9039 0.23(8) Uiso 1 1 calc R
H34B H 0.8298 0.4676 0.9304 0.24(9) Uiso 1 1 calc R
C35 C 0.8021(9) 0.3837(18) 1.0255(7) 0.135(5) Uani 1 1 d .
H35A H 0.7744 0.4576 1.0332 0.8(4) Uiso 1 1 calc R
H35B H 0.7613 0.3188 1.0240 1.1(5) Uiso 1 1 calc R
C101 C 0.8467(5) -0.2598(7) 1.0314(5) 0.0601(19) Uani 1 1 d .
H10A H 0.8083 -0.2989 0.9822 0.08(3) Uiso 1 1 calc R
H10B H 0.8322 -0.2857 1.0799 0.12(4) Uiso 1 1 calc R
H10C H 0.9080 -0.2789 1.0385 0.11(3) Uiso 1 1 calc R
C102 C 0.8694(5) -0.0439(8) 0.9326(5) 0.061(2) Uani 1 1 d .
H10D H 0.8622 0.0405 0.9278 0.07(3) Uiso 1 1 calc R
H10E H 0.8347 -0.0805 0.8807 0.09(3) Uiso 1 1 calc R
H10F H 0.9314 -0.0636 0.9446 0.12(4) Uiso 1 1 calc R
C103 C 0.9066(4) -0.0310(7) 1.1167(4) 0.0580(19) Uani 1 1 d .
H10G H 0.9017 0.0538 1.1127 0.049(19) Uiso 1 1 calc R
H10H H 0.9672 -0.0540 1.1239 0.07(2) Uiso 1 1 calc R
H10I H 0.8903 -0.0577 1.1640 0.08(3) Uiso 1 1 calc R
C201 C 0.7000(5) -0.2589(7) 0.8224(5) 0.0579(19) Uani 1 1 d .
H20A H 0.6937 -0.3201 0.8598 0.08(3) Uiso 1 1 calc R
H20B H 0.7608 -0.2313 0.8404 0.08(3) Uiso 1 1 calc R
H20C H 0.6848 -0.2899 0.7663 0.10(3) Uiso 1 1 calc R
C202 C 0.5108(5) -0.1979(7) 0.7819(5) 0.062(2) Uani 1 1 d .
H20D H 0.5035 -0.2586 0.8192 0.13(4) Uiso 1 1 calc R
H20E H 0.5024 -0.2315 0.7274 0.08(3) Uiso 1 1 calc R
H20F H 0.4673 -0.1366 0.7772 0.10(3) Uiso 1 1 calc R
C203 C 0.6376(7) -0.0167(7) 0.7522(4) 0.071(2) Uani 1 1 d .
H20G H 0.6964 0.0172 0.7743 0.10(4) Uiso 1 1 calc R
H20H H 0.5935 0.0438 0.7475 0.10(3) Uiso 1 1 calc R
H20I H 0.6298 -0.0499 0.6977 0.11(3) 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'
Dy Dy -0.1892 4.4098 '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 Dy O11 74.02(12) . .
O21 Dy Cl 104.61(9) . .
O11 Dy Cl 78.85(9) . .
O21 Dy C2 121.13(14) . 3_657
O11 Dy C2 156.05(14) . 3_657
Cl Dy C2 79.21(12) . 3_657
O21 Dy B4 131.56(15) . .
O11 Dy B4 80.15(16) . .
Cl Dy B4 109.69(13) . .
C2 Dy B4 98.40(16) 3_657 .
O21 Dy B3 98.19(15) . .
O11 Dy B3 77.98(15) . .
Cl Dy B3 141.34(13) . .
C2 Dy B3 114.66(16) 3_657 .
B4 Dy B3 35.71(17) . .
O21 Dy C1 88.84(14) . 3_657
O11 Dy C1 152.54(15) . 3_657
Cl Dy C1 85.15(12) . 3_657
C2 Dy C1 32.32(15) 3_657 3_657
B4 Dy C1 126.60(17) . 3_657
B3 Dy C1 126.56(17) . 3_657
O21 Dy B3 129.28(15) . 3_657
O11 Dy B3 150.92(15) . 3_657
Cl Dy B3 106.50(13) . 3_657
C2 Dy B3 33.59(16) 3_657 3_657
B4 Dy B3 71.09(17) . 3_657
B3 Dy B3 81.09(18) . 3_657
C1 Dy B3 55.56(17) 3_657 3_657
O21 Dy B5 72.50(16) . 3_657
O11 Dy B5 145.62(15) . 3_657
Cl Dy B5 117.16(14) . 3_657
C2 Dy B5 55.71(17) 3_657 3_657
B4 Dy B5 117.45(18) . 3_657
B3 Dy B5 99.20(18) . 3_657
C1 Dy B5 33.44(17) 3_657 3_657
B3 Dy B5 57.87(18) 3_657 3_657
O21 Dy B4 96.35(15) . 3_657
O11 Dy B4 145.23(15) . 3_657
Cl Dy B4 135.60(12) . 3_657
C2 Dy B4 56.52(16) 3_657 3_657
B4 Dy B4 82.31(18) . 3_657
B3 Dy B4 70.32(17) . 3_657
C1 Dy B4 56.25(17) 3_657 3_657
B3 Dy B4 35.33(16) 3_657 3_657
B5 Dy B4 35.16(17) 3_657 3_657
C101 Si1 C103 106.3(4) . .
C101 Si1 C102 110.2(4) . .
C103 Si1 C102 105.9(3) . .
C101 Si1 C1 113.2(3) . .
C103 Si1 C1 109.1(3) . .
C102 Si1 C1 111.7(3) . .
C201 Si2 C202 104.6(4) . .
C201 Si2 C203 109.2(4) . .
C202 Si2 C203 109.2(4) . .
C201 Si2 C2 117.9(3) . .
C202 Si2 C2 107.6(3) . .
C203 Si2 C2 108.1(3) . .
C2 C1 B5 111.2(4) . .
C2 C1 B6 64.7(3) . .
B5 C1 B6 65.8(4) . .
C2 C1 Si1 126.1(4) . .
B5 C1 Si1 120.4(4) . .
B6 C1 Si1 123.9(4) . .
C2 C1 Dy 73.4(3) . 3_657
B5 C1 Dy 73.5(3) . 3_657
B6 C1 Dy 101.9(3) . 3_657
Si1 C1 Dy 134.1(3) . 3_657
C1 C2 B3 110.8(4) . .
C1 C2 B6 63.5(3) . .
B3 C2 B6 65.8(4) . .
C1 C2 Si2 131.5(4) . .
B3 C2 Si2 115.8(4) . .
B6 C2 Si2 126.3(4) . .
C1 C2 Dy 74.2(3) . 3_657
B3 C2 Dy 73.6(3) . 3_657
B6 C2 Dy 101.8(3) . 3_657
Si2 C2 Dy 131.2(3) . 3_657
C2 B3 B4 106.6(4) . .
C2 B3 B6 61.6(3) . .
B4 B3 B6 62.4(3) . .
C2 B3 Dy 171.5(4) . .
B4 B3 Dy 72.1(3) . .
B6 B3 Dy 123.0(3) . .
C2 B3 Dy 72.8(3) . 3_657
B4 B3 Dy 74.0(3) . 3_657
B6 B3 Dy 99.6(3) . 3_657
Dy B3 Dy 98.91(18) . 3_657
B5 B4 B3 104.7(4) . .
B5 B4 B6 62.1(3) . .
B3 B4 B6 62.5(3) . .
B5 B4 Dy 168.5(4) . .
B3 B4 Dy 72.2(3) . .
B6 B4 Dy 123.1(3) . .
B5 B4 Dy 71.0(3) . 3_657
B3 B4 Dy 70.7(3) . 3_657
B6 B4 Dy 97.9(3) . 3_657
Dy B4 Dy 97.69(18) . 3_657
C1 B5 B4 106.6(4) . .
C1 B5 B6 61.2(4) . .
B4 B5 B6 62.8(3) . .
C1 B5 Dy 73.0(3) . 3_657
B4 B5 Dy 73.9(3) . 3_657
B6 B5 Dy 99.7(3) . 3_657
C1 B6 C2 51.8(3) . .
C1 B6 B5 53.0(3) . .
C2 B6 B5 92.1(4) . .
C1 B6 B4 94.7(4) . .
C2 B6 B4 94.4(4) . .
B5 B6 B4 55.1(3) . .
C1 B6 B3 92.1(4) . .
C2 B6 B3 52.6(3) . .
B5 B6 B3 94.4(4) . .
B4 B6 B3 55.1(3) . .
C15 O11 C12 108.9(4) . .
C15 O11 Dy 126.6(3) . .
C12 O11 Dy 123.5(3) . .
O11 C12 C13 106.1(5) . .
C12 C13 C14 103.6(5) . .
C15 C14 C13 102.4(5) . .
O11 C15 C14 105.3(5) . .
C22 O21 C25 109.0(4) . .
C22 O21 Dy 128.5(3) . .
C25 O21 Dy 121.3(3) . .
O21 C22 C23 104.5(4) . .
C22 C23 C24 102.0(5) . .
C25 C24 C23 104.1(5) . .
O21 C25 C24 105.9(5) . .
C32 O31 C35 112.2(10) . .
O31 C32 C33 110.1(12) . .
C34 C33 C32 104.5(11) . .
C33 C34 C35 106.6(11) . .
O31 C35 C34 102.8(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy O21 2.365(3) .
Dy O11 2.467(4) .
Dy Cl 2.5757(14) .
Dy C2 2.697(5) 3_657
Dy B4 2.706(6) .
Dy B3 2.706(6) .
Dy C1 2.707(5) 3_657
Dy B3 2.708(6) 3_657
Dy B5 2.714(6) 3_657
Dy B4 2.758(6) 3_657
Si1 C101 1.862(8) .
Si1 C103 1.870(7) .
Si1 C102 1.875(7) .
Si1 C1 1.880(5) .
Si2 C201 1.865(7) .
Si2 C202 1.866(7) .
Si2 C203 1.871(8) .
Si2 C2 1.881(5) .
C1 C2 1.504(7) .
C1 B5 1.559(8) .
C1 B6 1.711(8) .
C1 Dy 2.707(5) 3_657
C2 B3 1.562(8) .
C2 B6 1.729(8) .
C2 Dy 2.696(5) 3_657
B3 B4 1.659(8) .
B3 B6 1.794(8) .
B3 Dy 2.708(6) 3_657
B4 B5 1.653(8) .
B4 B6 1.792(8) .
B4 Dy 2.758(6) 3_657
B5 B6 1.781(8) .
B5 Dy 2.714(6) 3_657
O11 C15 1.457(6) .
O11 C12 1.461(7) .
C12 C13 1.498(9) .
C13 C14 1.518(9) .
C14 C15 1.502(8) .
O21 C22 1.460(6) .
O21 C25 1.462(7) .
C22 C23 1.505(8) .
C23 C24 1.514(9) .
C24 C25 1.488(9) .
O31 C32 1.269(14) .
O31 C35 1.448(14) .
C32 C33 1.483(16) .
C33 C34 1.417(15) .
C34 C35 1.485(13) .
