#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:27:31 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179791 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/87/7008798.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_7008798
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Huang, Qigu'
'Lappert, Michael F.'
'Zhou, Meisu'
_publ_section_title
;
 The coordination chemistry of the C1-symmetric bis(silyl)methyl ligand
 [CH(SiMe3){SiMe(OMe)2}]- revisited: Li/M- (M = Zn, Tl, Ce), Li4- or
 Ce2-methoxy-bridged alkyls.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2988
_journal_page_last               2993
_journal_paper_doi               10.1039/b508601a
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H60 Cl2 Li2 O8 Si4 Zn2'
_chemical_formula_sum            'C24 H60 Cl2 Li2 O8 Si4 Zn2'
_chemical_formula_weight         804.6
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-12-08T11:48:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.667(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6026(3)
_cell_length_b                   15.4505(3)
_cell_length_c                   13.7502(4)
_cell_measurement_reflns_used    10601
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     2033.28(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.633564E-1
_diffrn_orient_matrix_UB_12      0.259408E-1
_diffrn_orient_matrix_UB_13      -0.463473E-1
_diffrn_orient_matrix_UB_21      0.818389E-1
_diffrn_orient_matrix_UB_22      -0.98406E-2
_diffrn_orient_matrix_UB_23      0.48491E-1
_diffrn_orient_matrix_UB_31      0.143339E-1
_diffrn_orient_matrix_UB_32      -0.584746E-1
_diffrn_orient_matrix_UB_33      -0.287212E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17527
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.75
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_T_max  0.6704
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0368P)²+1.9864P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                3195
_reflns_number_total             3584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508601a.txt
_cod_data_source_block           (3)-dec1103
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7008798
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.04011(3) 0.437409(17) 0.924628(18) 0.02229(10) Uani 1 1 d . . .
Li Li -0.1831(4) 0.5588(3) 0.8527(3) 0.0308(9) Uani 1 1 d . . .
Cl Cl -0.17798(7) 0.40258(4) 0.85038(5) 0.03443(17) Uani 1 1 d . . .
Si1 Si 0.22897(8) 0.37587(5) 0.75442(5) 0.03465(19) Uani 1 1 d . . .
Si2 Si 0.30676(7) 0.33378(4) 0.97630(5) 0.02455(16) Uani 1 1 d . . .
O1 O -0.00861(16) 0.56658(10) 0.93082(11) 0.0221(3) Uani 1 1 d . . .
O2 O 0.18885(18) 0.26071(11) 0.99639(13) 0.0350(4) Uani 1 1 d . . .
O3 O 0.33542(17) 0.38624(12) 1.08269(12) 0.0316(4) Uani 1 1 d . . .
O4 O -0.2165(2) 0.59496(12) 0.71833(13) 0.0368(4) Uani 1 1 d . . .
C1 C 0.0843(3) 0.63007(16) 0.8968(2) 0.0333(6) Uani 1 1 d . . .
H1A H 0.1711 0.6307 0.9395 0.05 Uiso 1 1 calc R . .
H1B H 0.0402 0.6872 0.8974 0.05 Uiso 1 1 calc R . .
H1C H 0.1054 0.6158 0.8301 0.05 Uiso 1 1 calc R . .
C2 C 0.2309(3) 0.40703(16) 0.88396(18) 0.0273(5) Uani 1 1 d . . .
H2 H 0.2872 0.4614 0.8909 0.033 Uiso 1 1 calc R . .
C3 C 0.1270(5) 0.4547(3) 0.6743(3) 0.0909(17) Uani 1 1 d . . .
H3A H 0.1275 0.4364 0.6061 0.136 Uiso 1 1 calc R . .
H3B H 0.1694 0.5122 0.6822 0.136 Uiso 1 1 calc R . .
H3C H 0.0305 0.4569 0.6926 0.136 Uiso 1 1 calc R . .
C4 C 0.4087(3) 0.3711(2) 0.7097(2) 0.0455(7) Uani 1 1 d . . .
H4A H 0.4016 0.354 0.6409 0.068 Uiso 1 1 calc R . .
H4B H 0.4653 0.3286 0.7483 0.068 Uiso 1 1 calc R . .
H4C H 0.4528 0.4282 0.7168 0.068 Uiso 1 1 calc R . .
C5 C 0.1488(4) 0.2664(3) 0.7353(3) 0.0680(11) Uani 1 1 d . . .
H5A H 0.1484 0.2504 0.6663 0.102 Uiso 1 1 calc R . .
H5B H 0.0527 0.2675 0.7544 0.102 Uiso 1 1 calc R . .
H5C H 0.2033 0.2239 0.7753 0.102 Uiso 1 1 calc R . .
C6 C 0.4725(3) 0.2777(2) 0.9527(2) 0.0405(7) Uani 1 1 d . . .
H6A H 0.5439 0.3208 0.9405 0.061 Uiso 1 1 calc R . .
H6B H 0.4563 0.2401 0.8956 0.061 Uiso 1 1 calc R . .
H6C H 0.5044 0.2428 1.0097 0.061 Uiso 1 1 calc R . .
C7 C 0.2174(3) 0.18410(19) 1.0524(2) 0.0470(7) Uani 1 1 d . . .
H7A H 0.1313 0.1503 1.0546 0.07 Uiso 1 1 calc R . .
H7B H 0.2527 0.1999 1.1189 0.07 Uiso 1 1 calc R . .
H7C H 0.2877 0.1494 1.0222 0.07 Uiso 1 1 calc R . .
C8 C 0.4638(3) 0.4296(2) 1.1122(2) 0.0427(7) Uani 1 1 d . . .
H8A H 0.4575 0.4558 1.1766 0.064 Uiso 1 1 calc R . .
H8B H 0.481 0.4749 1.0647 0.064 Uiso 1 1 calc R . .
H8C H 0.5408 0.3878 1.1154 0.064 Uiso 1 1 calc R . .
C9 C -0.2498(4) 0.5378(2) 0.6373(2) 0.0571(10) Uani 1 1 d . . .
H9A H -0.2736 0.4794 0.6604 0.069 Uiso 1 1 calc R . .
H9B H -0.17 0.5329 0.5964 0.069 Uiso 1 1 calc R . .
C10 C -0.3725(4) 0.57808(19) 0.5811(2) 0.0513(8) Uani 1 1 d . . .
H10A H -0.4607 0.5637 0.61 0.062 Uiso 1 1 calc R . .
H10B H -0.3793 0.5593 0.512 0.062 Uiso 1 1 calc R . .
C11 C -0.3402(3) 0.67348(19) 0.5902(2) 0.0445(7) Uani 1 1 d . . .
H11A H -0.4269 0.7084 0.5848 0.053 Uiso 1 1 calc R . .
H11B H -0.2793 0.6925 0.5395 0.053 Uiso 1 1 calc R . .
C12 C -0.2654(3) 0.68078(16) 0.69130(19) 0.0345(6) Uani 1 1 d . . .
H12A H -0.1857 0.7214 0.6907 0.041 Uiso 1 1 calc R . .
H12B H -0.3301 0.7023 0.7383 0.041 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'
H H 0 0 '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'
Zn Zn 0.2839 1.4301 '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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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
_geom_angle_publ_flag
C2 Zn O1 118.35(8) . 3_567 ?
C2 Zn O1 116.97(9) . . ?
O1 Zn O1 86.36(6) 3_567 . ?
C2 Zn Cl 129.31(7) . . ?
O1 Zn Cl 102.85(5) 3_567 . ?
O1 Zn Cl 92.48(5) . . ?
O1 Li O4 125.9(2) . . ?
O1 Li O3 111.6(2) . 3_567 ?
O4 Li O3 103.6(2) . 3_567 ?
O1 Li Cl 93.03(16) . . ?
O4 Li Cl 106.17(19) . . ?
O3 Li Cl 117.1(2) 3_567 . ?
Zn Cl Li 77.32(10) . . ?
C2 Si1 C3 111.31(15) . . ?
C2 Si1 C5 110.11(14) . . ?
C3 Si1 C5 108.5(2) . . ?
C2 Si1 C4 112.87(13) . . ?
C3 Si1 C4 106.52(18) . . ?
C5 Si1 C4 107.31(16) . . ?
O2 Si2 O3 104.64(10) . . ?
O2 Si2 C2 107.76(11) . . ?
O3 Si2 C2 109.77(11) . . ?
O2 Si2 C6 108.70(12) . . ?
O3 Si2 C6 107.15(11) . . ?
C2 Si2 C6 118.01(12) . . ?
C1 O1 Li 113.56(19) . . ?
C1 O1 Zn 119.13(14) . 3_567 ?
Li O1 Zn 110.61(15) . 3_567 ?
C1 O1 Zn 120.18(15) . . ?
Li O1 Zn 96.15(14) . . ?
Zn O1 Zn 93.64(6) 3_567 . ?
C7 O2 Si2 123.91(17) . . ?
C8 O3 Si2 123.34(17) . . ?
C8 O3 Li 109.0(2) . 3_567 ?
Si2 O3 Li 121.89(15) . 3_567 ?
C9 O4 C12 108.47(19) . . ?
C9 O4 Li 125.0(2) . . ?
C12 O4 Li 122.46(19) . . ?
Si2 C2 Si1 119.11(14) . . ?
Si2 C2 Zn 105.92(12) . . ?
Si1 C2 Zn 113.03(12) . . ?
O4 C9 C10 105.2(2) . . ?
C9 C10 C11 102.5(3) . . ?
C10 C11 C12 103.2(2) . . ?
O4 C12 C11 106.7(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn C2 2.014(2) . ?
Zn O1 2.0356(16) 3_567 ?
Zn O1 2.0532(15) . ?
Zn Cl 2.3173(7) . ?
Li O1 1.919(4) . ?
Li O4 1.933(4) . ?
Li O3 1.965(5) 3_567 ?
Li Cl 2.414(4) . ?
Si1 C2 1.844(2) . ?
Si1 C3 1.865(4) . ?
Si1 C5 1.868(4) . ?
Si1 C4 1.880(3) . ?
Si2 O2 1.6382(19) . ?
Si2 O3 1.6755(18) . ?
Si2 C2 1.809(2) . ?
Si2 C6 1.863(3) . ?
O1 C1 1.430(3) . ?
O2 C7 1.427(3) . ?
O3 C8 1.432(3) . ?
O3 Li 1.965(5) 3_567 ?
O4 C9 1.437(3) . ?
O4 C12 1.445(3) . ?
C9 C10 1.491(4) . ?
C10 C11 1.509(4) . ?
C11 C12 1.516(4) . ?
