#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075405.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_4075405
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 Gd O3 Si2'
_chemical_formula_weight         626.69
_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                 108.977(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.946(4)
_cell_length_b                   11.442(3)
_cell_length_c                   16.990(4)
_cell_measurement_reflns_used    217
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      -14
_cell_volume                     2931.4(13)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10343
_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    2.453
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.473094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.00000(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.523
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.523
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.908
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+9.1656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                4971
_reflns_number_total             5053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060268ksi20060525_065827.cif
_cod_data_source_block           C9_hos218
_cod_original_cell_volume        2931.7(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075405
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
Gd Gd 0.418902(16) 0.14023(2) 0.946051(15) 0.02474(10) Uani 1 1 d .
Cl Cl 0.38250(11) 0.33822(12) 1.00257(10) 0.0454(4) Uani 1 1 d .
Si1 Si 0.83140(11) -0.09892(17) 1.01903(11) 0.0411(4) Uani 1 1 d .
Si2 Si 0.62518(11) -0.13283(16) 0.82342(10) 0.0385(4) Uani 1 1 d .
C1 C 0.7150(3) -0.0497(5) 1.0046(3) 0.0290(12) Uani 1 1 d .
C2 C 0.6363(3) -0.0641(5) 0.9273(3) 0.0273(11) Uani 1 1 d .
B3 B 0.5592(4) 0.0197(5) 0.9285(4) 0.0245(12) Uani 1 1 d .
H3 H 0.5113 0.0144 0.8644 0.041(17) Uiso 1 1 calc R
B4 B 0.5959(4) 0.0951(5) 1.0162(4) 0.0259(12) Uani 1 1 d .
H4 H 0.5911 0.1746 1.0519 0.12(4) Uiso 1 1 calc R
B5 B 0.6963(4) 0.0418(5) 1.0639(4) 0.0281(13) Uani 1 1 d .
H5 H 0.7438 0.0749 1.1231 0.015(12) Uiso 1 1 calc R
B6 B 0.6698(4) 0.0773(6) 0.9564(4) 0.0307(13) Uani 1 1 d .
H6 H 0.6976 0.1456 0.9257 0.045(17) Uiso 1 1 calc R
O11 O 0.4789(3) 0.2813(3) 0.8656(2) 0.0355(9) Uani 1 1 d .
C12 C 0.5340(5) 0.3813(6) 0.9034(4) 0.0508(18) Uani 1 1 d .
H12A H 0.5847 0.3562 0.9508 0.07(2) Uiso 1 1 calc R
H12B H 0.4996 0.4385 0.9231 0.07(2) Uiso 1 1 calc R
C13 C 0.5649(5) 0.4333(6) 0.8371(4) 0.0534(18) Uani 1 1 d .
H13A H 0.6253 0.4641 0.8606 0.050(19) Uiso 1 1 calc R
H13B H 0.5254 0.4964 0.8080 0.09(3) Uiso 1 1 calc R
C14 C 0.5620(5) 0.3316(6) 0.7791(4) 0.0488(16) Uani 1 1 d .
H14A H 0.5550 0.3588 0.7226 0.042(17) Uiso 1 1 calc R
H14B H 0.6157 0.2837 0.7993 0.10(3) Uiso 1 1 calc R
C15 C 0.4820(5) 0.2657(6) 0.7818(4) 0.0440(15) Uani 1 1 d .
H15A H 0.4282 0.2969 0.7408 0.08(3) Uiso 1 1 calc R
H15B H 0.4872 0.1827 0.7700 0.044(18) Uiso 1 1 calc R
O21 O 0.3229(2) 0.1284(3) 0.8052(2) 0.0324(8) Uani 1 1 d .
C22 C 0.3114(4) 0.0311(5) 0.7469(3) 0.0336(13) Uani 1 1 d .
H22A H 0.3252 -0.0435 0.7767 0.029(14) Uiso 1 1 calc R
H22B H 0.3497 0.0404 0.7124 0.040(17) Uiso 1 1 calc R
C23 C 0.2152(4) 0.0366(6) 0.6947(4) 0.0455(16) Uani 1 1 d .
H23A H 0.1776 -0.0025 0.7222 0.050(19) Uiso 1 1 calc R
H23B H 0.2052 0.0012 0.6398 0.051(19) Uiso 1 1 calc R
C24 C 0.1980(5) 0.1667(6) 0.6877(4) 0.0548(18) Uani 1 1 d .
H24A H 0.2171 0.2009 0.6435 0.09(3) Uiso 1 1 calc R
H24B H 0.1349 0.1836 0.6764 0.08(3) Uiso 1 1 calc R
C25 C 0.2519(4) 0.2124(6) 0.7705(4) 0.0479(16) Uani 1 1 d .
H25A H 0.2764 0.2892 0.7647 0.06(2) Uiso 1 1 calc R
H25B H 0.2153 0.2202 0.8068 0.07(2) Uiso 1 1 calc R
O31 O 0.8863(7) 0.3687(10) 1.0907(5) 0.149(4) Uani 1 1 d .
C32 C 0.9455(13) 0.336(2) 1.0616(8) 0.183(9) Uani 1 1 d .
H32A H 0.9665 0.2583 1.0828 0.26(11) Uiso 1 1 calc R
H32B H 0.9960 0.3902 1.0799 0.37(18) Uiso 1 1 calc R
C33 C 0.9106(10) 0.334(2) 0.9688(8) 0.145(6) Uani 1 1 d .
H33A H 0.9496 0.3770 0.9449 0.32(13) Uiso 1 1 calc R
H33B H 0.9050 0.2530 0.9481 0.42(19) Uiso 1 1 calc R
C34 C 0.8276(7) 0.3870(15) 0.9490(7) 0.111(4) Uani 1 1 d .
H34A H 0.7840 0.3448 0.9037 0.19(7) Uiso 1 1 calc R
H34B H 0.8308 0.4679 0.9312 0.20(8) Uiso 1 1 calc R
C35 C 0.8023(10) 0.3838(18) 1.0252(7) 0.138(6) Uani 1 1 d .
H35A H 0.7735 0.4568 1.0323 0.4(2) Uiso 1 1 calc R
H35B H 0.7623 0.3183 1.0238 2.0(16) Uiso 1 1 calc R
C101 C 0.8464(5) -0.2600(7) 1.0311(5) 0.062(2) Uani 1 1 d .
H10A H 0.8078 -0.2986 0.9818 0.13(4) Uiso 1 1 calc R
H10B H 0.8315 -0.2854 1.0794 0.12(4) Uiso 1 1 calc R
H10C H 0.9076 -0.2798 1.0385 0.12(4) Uiso 1 1 calc R
C102 C 0.8705(5) -0.0446(8) 0.9327(5) 0.062(2) Uani 1 1 d .
H10D H 0.8633 0.0396 0.9280 0.08(3) Uiso 1 1 calc R
H10E H 0.8358 -0.0810 0.8808 0.08(3) Uiso 1 1 calc R
H10F H 0.9326 -0.0642 0.9448 0.10(3) Uiso 1 1 calc R
C103 C 0.9075(4) -0.0331(7) 1.1167(4) 0.0570(19) Uani 1 1 d .
H10G H 0.9030 0.0514 1.1132 0.047(19) Uiso 1 1 calc R
H10H H 0.9680 -0.0565 1.1238 0.07(2) Uiso 1 1 calc R
H10I H 0.8911 -0.0602 1.1638 0.07(2) Uiso 1 1 calc R
C201 C 0.7000(5) -0.2574(7) 0.8214(5) 0.0566(19) Uani 1 1 d .
H20A H 0.6936 -0.3184 0.8587 0.07(3) Uiso 1 1 calc R
H20B H 0.7610 -0.2304 0.8392 0.08(3) Uiso 1 1 calc R
H20C H 0.6843 -0.2882 0.7653 0.09(3) Uiso 1 1 calc R
C202 C 0.5113(5) -0.1950(8) 0.7810(5) 0.063(2) Uani 1 1 d .
H20D H 0.5037 -0.2556 0.8180 0.16(6) Uiso 1 1 calc R
H20E H 0.5029 -0.2281 0.7264 0.08(3) Uiso 1 1 calc R
H20F H 0.4680 -0.1336 0.7764 0.10(3) Uiso 1 1 calc R
C203 C 0.6393(7) -0.0150(7) 0.7522(5) 0.071(3) Uani 1 1 d .
H20G H 0.6982 0.0184 0.7746 0.13(5) Uiso 1 1 calc R
H20H H 0.5953 0.0455 0.7472 0.09(3) Uiso 1 1 calc R
H20I H 0.6317 -0.0480 0.6977 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'
Gd Gd -0.1653 3.9035 '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 Gd O11 73.90(13) . .
O21 Gd Cl 105.79(10) . .
O11 Gd Cl 79.06(10) . .
O21 Gd C2 120.52(14) . 3_657
O11 Gd C2 156.93(14) . 3_657
Cl Gd C2 79.52(12) . 3_657
O21 Gd B3 98.23(15) . .
O11 Gd B3 78.07(15) . .
Cl Gd B3 140.48(13) . .
C2 Gd B3 114.39(16) 3_657 .
O21 Gd B4 131.37(15) . .
O11 Gd B4 80.57(16) . .
Cl Gd B4 109.07(13) . .
C2 Gd B4 98.53(16) 3_657 .
B3 Gd B4 35.31(17) . .
O21 Gd C1 88.64(15) . 3_657
O11 Gd C1 152.56(15) . 3_657
Cl Gd C1 85.79(12) . 3_657
C2 Gd C1 31.93(15) 3_657 3_657
B3 Gd C1 126.25(17) . 3_657
B4 Gd C1 126.31(17) . 3_657
O21 Gd B3 128.23(15) . 3_657
O11 Gd B3 151.81(15) . 3_657
Cl Gd B3 106.36(13) . 3_657
C2 Gd B3 33.28(16) 3_657 3_657
B3 Gd B3 81.13(17) . 3_657
B4 Gd B3 71.48(17) . 3_657
C1 Gd B3 54.88(16) 3_657 3_657
O21 Gd B5 72.39(16) . 3_657
O11 Gd B5 145.48(15) . 3_657
Cl Gd B5 117.31(14) . 3_657
C2 Gd B5 54.81(17) 3_657 3_657
B3 Gd B5 99.55(18) . 3_657
B4 Gd B5 117.31(18) . 3_657
C1 Gd B5 32.79(17) 3_657 3_657
B3 Gd B5 57.02(17) 3_657 3_657
O21 Gd B4 95.79(15) . 3_657
O11 Gd B4 145.47(15) . 3_657
Cl Gd B4 135.17(13) . 3_657
C2 Gd B4 55.73(16) 3_657 3_657
B3 Gd B4 70.81(17) . 3_657
B4 Gd B4 82.54(18) . 3_657
C1 Gd B4 55.45(17) 3_657 3_657
B3 Gd B4 34.77(16) 3_657 3_657
B5 Gd B4 34.79(17) 3_657 3_657
C101 Si1 C103 106.1(4) . .
C101 Si1 C102 110.6(4) . .
C103 Si1 C102 106.0(3) . .
C101 Si1 C1 113.4(3) . .
C103 Si1 C1 108.9(3) . .
C102 Si1 C1 111.3(3) . .
C202 Si2 C201 104.5(4) . .
C202 Si2 C203 109.3(4) . .
C201 Si2 C203 109.0(4) . .
C202 Si2 C2 107.7(3) . .
C201 Si2 C2 118.0(3) . .
C203 Si2 C2 108.1(3) . .
C2 C1 B5 111.2(4) . .
C2 C1 B6 64.7(3) . .
B5 C1 B6 66.2(4) . .
C2 C1 Si1 126.2(4) . .
B5 C1 Si1 120.6(4) . .
B6 C1 Si1 124.2(4) . .
C2 C1 Gd 73.4(3) . 3_657
B5 C1 Gd 73.9(3) . 3_657
B6 C1 Gd 102.7(3) . 3_657
Si1 C1 Gd 133.0(3) . 3_657
C1 C2 B3 110.9(4) . .
C1 C2 B6 63.4(4) . .
B3 C2 B6 66.0(4) . .
C1 C2 Si2 131.4(4) . .
B3 C2 Si2 115.6(4) . .
B6 C2 Si2 125.8(4) . .
C1 C2 Gd 74.7(3) . 3_657
B3 C2 Gd 74.2(3) . 3_657
B6 C2 Gd 102.9(3) . 3_657
Si2 C2 Gd 130.6(3) . 3_657
C2 B3 B4 106.4(4) . .
C2 B3 B6 61.3(3) . .
B4 B3 B6 62.7(3) . .
C2 B3 Gd 171.1(4) . .
B4 B3 Gd 72.6(3) . .
B6 B3 Gd 123.8(3) . .
C2 B3 Gd 72.5(3) . 3_657
B4 B3 Gd 74.3(3) . 3_657
B6 B3 Gd 100.0(3) . 3_657
Gd B3 Gd 98.87(17) . 3_657
B3 B4 B5 104.6(4) . .
B3 B4 B6 62.5(3) . .
B5 B4 B6 61.9(4) . .
B3 B4 Gd 72.1(3) . .
B5 B4 Gd 168.3(4) . .
B6 B4 Gd 123.2(3) . .
B3 B4 Gd 70.9(3) . 3_657
B5 B4 Gd 71.0(3) . 3_657
B6 B4 Gd 98.1(3) . 3_657
Gd B4 Gd 97.46(18) . 3_657
C1 B5 B4 106.9(5) . .
C1 B5 B6 61.2(4) . .
B4 B5 B6 63.0(4) . .
C1 B5 Gd 73.4(3) . 3_657
B4 B5 Gd 74.2(3) . 3_657
B6 B5 Gd 100.3(3) . 3_657
C1 B6 C2 51.9(3) . .
C1 B6 B5 52.6(3) . .
C2 B6 B5 91.6(4) . .
C1 B6 B3 92.3(4) . .
C2 B6 B3 52.7(3) . .
B5 B6 B3 94.1(4) . .
C1 B6 B4 94.4(4) . .
C2 B6 B4 94.0(4) . .
B5 B6 B4 55.1(3) . .
B3 B6 B4 54.8(3) . .
C15 O11 C12 108.7(4) . .
C15 O11 Gd 126.8(3) . .
C12 O11 Gd 123.3(3) . .
O11 C12 C13 106.2(5) . .
C12 C13 C14 103.7(5) . .
C15 C14 C13 102.3(5) . .
O11 C15 C14 105.6(5) . .
C25 O21 C22 108.6(4) . .
C25 O21 Gd 122.0(3) . .
C22 O21 Gd 128.3(3) . .
O21 C22 C23 104.3(5) . .
C22 C23 C24 102.2(5) . .
C25 C24 C23 103.8(5) . .
O21 C25 C24 106.6(5) . .
C32 O31 C35 111.0(11) . .
O31 C32 C33 110.6(13) . .
C34 C33 C32 104.1(12) . .
C33 C34 C35 106.6(11) . .
O31 C35 C34 103.2(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd O21 2.389(3) .
Gd O11 2.498(4) .
Gd Cl 2.5988(15) .
Gd C2 2.720(5) 3_657
Gd B3 2.726(6) .
Gd B4 2.733(6) .
Gd C1 2.739(5) 3_657
Gd B3 2.744(6) 3_657
Gd B5 2.746(6) 3_657
Gd B4 2.795(6) 3_657
Si1 C101 1.861(8) .
Si1 C103 1.866(7) .
Si1 C102 1.876(7) .
Si1 C1 1.879(5) .
Si2 C202 1.863(7) .
Si2 C201 1.866(7) .
Si2 C203 1.874(8) .
Si2 C2 1.886(5) .
C1 C2 1.501(7) .
C1 B5 1.548(8) .
C1 B6 1.707(8) .
C1 Gd 2.739(5) 3_657
C2 B3 1.565(8) .
C2 B6 1.725(8) .
C2 Gd 2.720(5) 3_657
B3 B4 1.656(8) .
B3 B6 1.797(8) .
B3 Gd 2.744(6) 3_657
B4 B5 1.657(8) .
B4 B6 1.801(8) .
B4 Gd 2.795(6) 3_657
B5 B6 1.783(8) .
B5 Gd 2.746(6) 3_657
O11 C15 1.451(7) .
O11 C12 1.459(7) .
C12 C13 1.492(9) .
C13 C14 1.516(10) .
C14 C15 1.496(9) .
O21 C25 1.456(7) .
O21 C22 1.462(6) .
C22 C23 1.503(8) .
C23 C24 1.512(9) .
C24 C25 1.484(9) .
O31 C32 1.256(15) .
O31 C35 1.447(15) .
C32 C33 1.492(17) .
C33 C34 1.396(15) .
C34 C35 1.477(14) .
