#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075409.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_4075409
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 Er O3 Si2'
_chemical_formula_weight         636.70
_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                 108.959(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.948(3)
_cell_length_b                   11.377(2)
_cell_length_c                   16.973(3)
_cell_measurement_reflns_used    749
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2912.5(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0175
_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            18841
_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    3.074
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.479436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.00004(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.434
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.434
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.576
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+7.6290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                5072
_reflns_number_total             5136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060268ksi20060525_065827.cif
_cod_data_source_block           C13_hos220
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075409
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
Er Er 0.419819(12) 0.137059(16) 0.946584(11) 0.02592(8) Uani 1 1 d .
Cl Cl 0.38020(9) 0.33343(10) 0.99841(8) 0.0445(3) Uani 1 1 d .
Si1 Si 0.82998(9) -0.09747(14) 1.01918(9) 0.0424(3) Uani 1 1 d .
Si2 Si 0.62396(9) -0.13541(13) 0.82421(8) 0.0396(3) Uani 1 1 d .
C1 C 0.7130(3) -0.0503(4) 1.0047(3) 0.0305(10) Uani 1 1 d .
C2 C 0.6341(3) -0.0653(4) 0.9278(3) 0.0282(9) Uani 1 1 d .
B3 B 0.5572(3) 0.0182(4) 0.9283(3) 0.0262(10) Uani 1 1 d .
H3 H 0.5098 0.0121 0.8640 0.046(14) Uiso 1 1 calc R
B4 B 0.5932(3) 0.0946(4) 1.0161(3) 0.0273(10) Uani 1 1 d .
H4 H 0.5877 0.1746 1.0516 0.11(3) Uiso 1 1 calc R
B5 B 0.6941(3) 0.0422(4) 1.0642(3) 0.0292(11) Uani 1 1 d .
H5 H 0.7416 0.0759 1.1233 0.026(11) Uiso 1 1 calc R
B6 B 0.6673(3) 0.0764(4) 0.9566(3) 0.0306(11) Uani 1 1 d .
H6 H 0.6950 0.1451 0.9257 0.042(13) Uiso 1 1 calc R
O11 O 0.4803(2) 0.2770(3) 0.86834(19) 0.0356(7) Uani 1 1 d .
C12 C 0.5352(4) 0.3778(5) 0.9068(3) 0.0537(15) Uani 1 1 d .
H12A H 0.5868 0.3522 0.9532 0.066(19) Uiso 1 1 calc R
H12B H 0.5010 0.4338 0.9280 0.064(19) Uiso 1 1 calc R
C13 C 0.5640(4) 0.4332(5) 0.8397(4) 0.0541(15) Uani 1 1 d .
H13A H 0.6239 0.4660 0.8625 0.053(16) Uiso 1 1 calc R
H13B H 0.5231 0.4957 0.8112 0.066(19) Uiso 1 1 calc R
C14 C 0.5620(4) 0.3319(5) 0.7809(4) 0.0509(14) Uani 1 1 d .
H14A H 0.5542 0.3599 0.7244 0.052(15) Uiso 1 1 calc R
H14B H 0.6163 0.2847 0.8006 0.062(18) Uiso 1 1 calc R
C15 C 0.4825(4) 0.2634(5) 0.7843(3) 0.0425(12) Uani 1 1 d .
H15A H 0.4281 0.2946 0.7440 0.065(18) Uiso 1 1 calc R
H15B H 0.4882 0.1803 0.7718 0.039(13) Uiso 1 1 calc R
O21 O 0.3262(2) 0.1281(3) 0.80885(18) 0.0325(7) Uani 1 1 d .
C22 C 0.3136(3) 0.0317(4) 0.7492(3) 0.0341(10) Uani 1 1 d .
H22A H 0.3259 -0.0442 0.7780 0.033(12) Uiso 1 1 calc R
H22B H 0.3525 0.0409 0.7152 0.035(13) Uiso 1 1 calc R
C23 C 0.2180(3) 0.0403(5) 0.6964(3) 0.0443(12) Uani 1 1 d .
H23A H 0.1794 0.0010 0.7229 0.051(16) Uiso 1 1 calc R
H23B H 0.2080 0.0061 0.6411 0.043(14) Uiso 1 1 calc R
C24 C 0.2027(4) 0.1714(5) 0.6913(4) 0.0528(15) Uani 1 1 d .
H24A H 0.2238 0.2066 0.6484 0.056(17) Uiso 1 1 calc R
H24B H 0.1397 0.1898 0.6787 0.09(2) Uiso 1 1 calc R
C25 C 0.2553(4) 0.2142(5) 0.7757(3) 0.0458(13) Uani 1 1 d .
H25A H 0.2802 0.2921 0.7722 0.066(18) Uiso 1 1 calc R
H25B H 0.2181 0.2195 0.8115 0.069(19) Uiso 1 1 calc R
O31 O 0.8857(6) 0.3667(8) 1.0910(4) 0.148(3) Uani 1 1 d .
C32 C 0.9483(10) 0.3378(18) 1.0622(7) 0.157(6) Uani 1 1 d .
H32A H 0.9721 0.2606 1.0840 0.27(9) Uiso 1 1 calc R
H32B H 0.9964 0.3954 1.0799 0.35(14) Uiso 1 1 calc R
C33 C 0.9117(8) 0.3337(16) 0.9690(6) 0.137(4) Uani 1 1 d .
H33A H 0.9498 0.3776 0.9443 0.27(9) Uiso 1 1 calc R
H33B H 0.9069 0.2524 0.9491 0.38(14) Uiso 1 1 calc R
C34 C 0.8270(6) 0.3864(12) 0.9484(5) 0.107(3) Uani 1 1 d .
H34A H 0.7838 0.3424 0.9037 0.19(6) Uiso 1 1 calc R
H34B H 0.8290 0.4675 0.9297 0.22(7) Uiso 1 1 calc R
C35 C 0.8022(7) 0.3838(14) 1.0253(6) 0.130(4) Uani 1 1 d .
H35A H 0.7744 0.4579 1.0327 0.6(2) Uiso 1 1 calc R
H35B H 0.7613 0.3189 1.0238 2.0(13) Uiso 1 1 calc R
C101 C 0.8470(4) -0.2599(5) 1.0316(4) 0.0604(16) Uani 1 1 d .
H10A H 0.8086 -0.2994 0.9825 0.08(2) Uiso 1 1 calc R
H10B H 0.8330 -0.2860 1.0803 0.12(3) Uiso 1 1 calc R
H10C H 0.9084 -0.2785 1.0385 0.10(3) Uiso 1 1 calc R
C102 C 0.8680(4) -0.0422(7) 0.9322(4) 0.0607(17) Uani 1 1 d .
H10D H 0.8607 0.0424 0.9277 0.07(2) Uiso 1 1 calc R
H10E H 0.8330 -0.0786 0.8803 0.09(2) Uiso 1 1 calc R
H10F H 0.9301 -0.0618 0.9438 0.10(3) Uiso 1 1 calc R
C103 C 0.9058(3) -0.0297(6) 1.1166(4) 0.0571(16) Uani 1 1 d .
H10G H 0.9008 0.0552 1.1126 0.054(17) Uiso 1 1 calc R
H10H H 0.9664 -0.0527 1.1240 0.069(19) Uiso 1 1 calc R
H10I H 0.8895 -0.0564 1.1640 0.07(2) Uiso 1 1 calc R
C201 C 0.7001(4) -0.2594(6) 0.8229(4) 0.0571(16) Uani 1 1 d .
H20A H 0.6940 -0.3209 0.8602 0.08(2) Uiso 1 1 calc R
H20B H 0.7608 -0.2313 0.8410 0.09(2) Uiso 1 1 calc R
H20C H 0.6851 -0.2905 0.7668 0.08(2) Uiso 1 1 calc R
C202 C 0.5100(4) -0.1988(6) 0.7824(4) 0.0616(17) Uani 1 1 d .
H20D H 0.5028 -0.2594 0.8199 0.12(3) Uiso 1 1 calc R
H20E H 0.5015 -0.2327 0.7279 0.07(2) Uiso 1 1 calc R
H20F H 0.4666 -0.1373 0.7777 0.10(3) Uiso 1 1 calc R
C203 C 0.6367(6) -0.0180(6) 0.7519(4) 0.071(2) Uani 1 1 d .
H20G H 0.6955 0.0162 0.7737 0.10(3) Uiso 1 1 calc R
H20H H 0.5925 0.0426 0.7469 0.11(3) Uiso 1 1 calc R
H20I H 0.6288 -0.0518 0.6975 0.12(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'
Er Er -0.2586 4.9576 '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 Er O11 73.90(11) . .
O21 Er Cl 103.54(8) . .
O11 Er Cl 78.72(8) . .
O21 Er C2 121.29(12) . 3_657
O11 Er C2 155.76(12) . 3_657
Cl Er C2 79.19(10) . 3_657
O21 Er B4 131.91(13) . .
O11 Er B4 79.91(13) . .
Cl Er B4 109.99(11) . .
C2 Er B4 98.48(14) 3_657 .
O21 Er B3 98.21(13) . .
O11 Er B3 77.58(13) . .
Cl Er B3 141.71(11) . .
C2 Er B3 115.23(14) 3_657 .
B4 Er B3 36.12(14) . .
O21 Er B3 129.83(13) . 3_657
O11 Er B3 150.74(13) . 3_657
Cl Er B3 106.70(11) . 3_657
C2 Er B3 33.66(14) 3_657 3_657
B4 Er B3 71.18(15) . 3_657
B3 Er B3 81.59(15) . 3_657
O21 Er B5 72.63(13) . 3_657
O11 Er B5 145.64(13) . 3_657
Cl Er B5 116.62(12) . 3_657
C2 Er B5 55.88(14) 3_657 3_657
B4 Er B5 118.06(15) . 3_657
B3 Er B5 99.73(15) . 3_657
B3 Er B5 58.26(15) 3_657 3_657
O21 Er C1 88.90(12) . 3_657
O11 Er C1 152.36(12) . 3_657
Cl Er C1 84.71(10) . 3_657
C2 Er C1 32.41(13) 3_657 3_657
B4 Er C1 126.92(14) . 3_657
B3 Er C1 127.18(14) . 3_657
B3 Er C1 55.80(14) 3_657 3_657
B5 Er C1 33.48(14) 3_657 3_657
O21 Er B4 96.78(13) . 3_657
O11 Er B4 145.15(13) . 3_657
Cl Er B4 135.85(11) . 3_657
C2 Er B4 56.82(14) 3_657 3_657
B4 Er B4 82.47(16) . 3_657
B3 Er B4 70.53(14) . 3_657
B3 Er B4 35.57(14) 3_657 3_657
B5 Er B4 35.60(15) 3_657 3_657
C1 Er B4 56.66(14) 3_657 3_657
C101 Si1 C103 106.2(3) . .
C101 Si1 C102 110.3(3) . .
C103 Si1 C102 106.0(3) . .
C101 Si1 C1 113.5(2) . .
C103 Si1 C1 109.1(2) . .
C102 Si1 C1 111.2(2) . .
C201 Si2 C202 105.1(3) . .
C201 Si2 C203 108.8(3) . .
C202 Si2 C203 109.1(4) . .
C201 Si2 C2 118.1(2) . .
C202 Si2 C2 107.2(2) . .
C203 Si2 C2 108.4(3) . .
C2 C1 B5 111.0(4) . .
C2 C1 B6 64.6(3) . .
B5 C1 B6 66.1(3) . .
C2 C1 Si1 126.7(3) . .
B5 C1 Si1 120.1(3) . .
B6 C1 Si1 123.9(3) . .
C2 C1 Er 72.9(2) . 3_657
B5 C1 Er 73.2(2) . 3_657
B6 C1 Er 101.5(3) . 3_657
Si1 C1 Er 134.4(2) . 3_657
C1 C2 B3 111.5(4) . .
C1 C2 B6 63.4(3) . .
B3 C2 B6 66.1(3) . .
C1 C2 Si2 130.7(3) . .
B3 C2 Si2 115.7(3) . .
B6 C2 Si2 126.0(3) . .
C1 C2 Er 74.7(2) . 3_657
B3 C2 Er 73.9(2) . 3_657
B6 C2 Er 102.0(2) . 3_657
Si2 C2 Er 131.4(2) . 3_657
C2 B3 B4 106.4(4) . .
C2 B3 B6 61.3(3) . .
B4 B3 B6 62.7(3) . .
C2 B3 Er 170.6(3) . .
B4 B3 Er 71.8(2) . .
B6 B3 Er 123.4(3) . .
C2 B3 Er 72.4(2) . 3_657
B4 B3 Er 73.5(2) . 3_657
B6 B3 Er 99.2(3) . 3_657
Er B3 Er 98.41(15) . 3_657
B3 B4 B5 104.5(4) . .
B3 B4 B6 62.2(3) . .
B5 B4 B6 61.7(3) . .
B3 B4 Er 72.1(2) . .
B5 B4 Er 168.4(3) . .
B6 B4 Er 123.1(3) . .
B3 B4 Er 70.9(2) . 3_657
B5 B4 Er 71.0(2) . 3_657
B6 B4 Er 97.6(3) . 3_657
Er B4 Er 97.53(16) . 3_657
C1 B5 B4 106.6(4) . .
C1 B5 B6 60.9(3) . .
B4 B5 B6 63.0(3) . .
C1 B5 Er 73.3(2) . 3_657
B4 B5 Er 73.4(2) . 3_657
B6 B5 Er 99.4(3) . 3_657
C1 B6 C2 52.1(3) . .
C1 B6 B5 53.1(3) . .
C2 B6 B5 92.1(3) . .
C1 B6 B3 92.7(3) . .
C2 B6 B3 52.6(3) . .
B5 B6 B3 94.8(3) . .
C1 B6 B4 94.9(3) . .
C2 B6 B4 94.1(3) . .
B5 B6 B4 55.3(3) . .
B3 B6 B4 55.1(3) . .
C15 O11 C12 108.7(4) . .
C15 O11 Er 127.1(3) . .
C12 O11 Er 123.3(3) . .
O11 C12 C13 106.1(4) . .
C12 C13 C14 103.5(4) . .
C15 C14 C13 101.9(4) . .
O11 C15 C14 105.9(4) . .
C22 O21 C25 108.7(3) . .
C22 O21 Er 128.8(2) . .
C25 O21 Er 121.3(3) . .
O21 C22 C23 104.5(4) . .
C22 C23 C24 102.2(4) . .
C25 C24 C23 103.8(4) . .
O21 C25 C24 106.0(4) . .
C32 O31 C35 112.0(8) . .
O31 C32 C33 108.9(10) . .
C34 C33 C32 105.2(9) . .
C33 C34 C35 106.3(9) . .
O31 C35 C34 103.9(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Er O21 2.331(3) .
Er O11 2.461(3) .
Er Cl 2.5544(12) .
Er C2 2.673(4) 3_657
Er B4 2.674(5) .
Er B3 2.677(5) .
Er B3 2.695(5) 3_657
Er B5 2.697(5) 3_657
Er C1 2.699(4) 3_657
Er B4 2.734(5) 3_657
Si1 C101 1.869(6) .
Si1 C103 1.869(6) .
Si1 C102 1.877(6) .
Si1 C1 1.879(5) .
Si2 C201 1.866(6) .
Si2 C202 1.867(6) .
Si2 C203 1.870(6) .
Si2 C2 1.889(4) .
C1 C2 1.499(6) .
C1 B5 1.554(7) .
C1 B6 1.699(7) .
C1 Er 2.699(4) 3_657
C2 B3 1.554(6) .
C2 B6 1.717(6) .
C2 Er 2.673(4) 3_657
B3 B4 1.659(7) .
B3 B6 1.789(7) .
B3 Er 2.695(5) 3_657
B4 B5 1.661(7) .
B4 B6 1.798(7) .
B4 Er 2.734(5) 3_657
B5 B6 1.778(7) .
B5 Er 2.697(5) 3_657
O11 C15 1.446(5) .
O11 C12 1.462(6) .
C12 C13 1.500(7) .
C13 C14 1.517(8) .
C14 C15 1.505(7) .
O21 C22 1.461(5) .
O21 C25 1.463(6) .
C22 C23 1.500(6) .
C23 C24 1.510(7) .
C24 C25 1.487(7) .
O31 C32 1.288(12) .
O31 C35 1.445(12) .
C32 C33 1.499(13) .
C33 C34 1.413(12) .
C34 C35 1.481(11) .
