#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:15:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179101 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/63/4306344.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_4306344
loop_
_publ_author_name
'David S. Kuiper'
'Peter T. Wolczanski'
'Emil B. Lobkovsky'
'Thomas R. Cundari'
_publ_section_title
;
Four-Coordinate Mo(II) as (silox)2Mo(PMe3)2 and Its W(IV) Congener
(silox)2HW(η2-CH2PMe2)(PMe3) (silox =tBu3SiO)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10542
_journal_page_last               10553
_journal_paper_doi               10.1021/ic8011958
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C28 H62 Cl3 Mo O3 Si2'
_chemical_formula_sum            'C28 H62 Cl3 Mo O3 Si2'
_chemical_formula_weight         705.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.374(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7262(8)
_cell_length_b                   15.4639(17)
_cell_length_c                   27.145(2)
_cell_measurement_reflns_used    2877
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.62
_cell_measurement_theta_min      2.63
_cell_volume                     3640.3(6)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14811
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.9060
_exptl_absorpt_correction_T_min  0.6887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         4409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0399P)²+0.2684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                3302
_reflns_number_total             4409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8011958_si_001_1.cif
_cod_data_source_block           dk16
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4306344
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Mo1 Mo 0.5000 0.300859(15) 0.2500 0.01361(6) Uani 1 2 d S . .
Cl1 Cl 0.76914(5) 0.29132(3) 0.273503(17) 0.01790(11) Uani 1 1 d . . .
Cl2 Cl 0.5000 0.45236(4) 0.2500 0.02180(16) Uani 1 2 d S . .
Si1 Si 0.54000(6) 0.31447(3) 0.122154(19) 0.01487(12) Uani 1 1 d . . .
O1 O 0.52950(13) 0.30146(8) 0.18412(4) 0.0143(3) Uani 1 1 d . . .
O2 O 0.5000 0.16069(11) 0.2500 0.0132(4) Uani 1 2 d S . .
C1 C 0.4393(2) 0.42128(13) 0.10166(7) 0.0228(5) Uani 1 1 d . . .
C2 C 0.5388(2) 0.50117(14) 0.11702(8) 0.0320(6) Uani 1 1 d . . .
H2A H 0.4806 0.5538 0.1073 0.048 Uiso 1 1 calc R . .
H2B H 0.6331 0.4997 0.1005 0.048 Uiso 1 1 calc R . .
H2C H 0.5662 0.5009 0.1530 0.048 Uiso 1 1 calc R . .
C3 C 0.2868(2) 0.43299(14) 0.12499(8) 0.0295(5) Uani 1 1 d . . .
H3A H 0.2366 0.4867 0.1127 0.044 Uiso 1 1 calc R . .
H3B H 0.3088 0.4358 0.1611 0.044 Uiso 1 1 calc R . .
H3C H 0.2184 0.3839 0.1159 0.044 Uiso 1 1 calc R . .
C4 C 0.4014(2) 0.42349(15) 0.04471(8) 0.0338(6) Uani 1 1 d . . .
H4A H 0.3309 0.3760 0.0342 0.051 Uiso 1 1 calc R . .
H4B H 0.4967 0.4171 0.0291 0.051 Uiso 1 1 calc R . .
H4C H 0.3526 0.4788 0.0348 0.051 Uiso 1 1 calc R . .
C5 C 0.4348(2) 0.21518(13) 0.09210(7) 0.0197(5) Uani 1 1 d . . .
C6 C 0.2588(2) 0.22395(15) 0.08907(8) 0.0279(5) Uani 1 1 d . . .
H6A H 0.2104 0.1703 0.0760 0.042 Uiso 1 1 calc R . .
H6B H 0.2248 0.2721 0.0671 0.042 Uiso 1 1 calc R . .
H6C H 0.2289 0.2350 0.1222 0.042 Uiso 1 1 calc R . .
C7 C 0.4790(2) 0.19805(14) 0.03932(7) 0.0293(5) Uani 1 1 d . . .
H7A H 0.5892 0.1845 0.0412 0.044 Uiso 1 1 calc R . .
H7B H 0.4569 0.2497 0.0188 0.044 Uiso 1 1 calc R . .
H7C H 0.4189 0.1492 0.0246 0.044 Uiso 1 1 calc R . .
C8 C 0.4745(2) 0.13417(13) 0.12339(7) 0.0234(5) Uani 1 1 d . . .
H8A H 0.4371 0.1410 0.1559 0.035 Uiso 1 1 calc R . .
H8B H 0.5865 0.1260 0.1277 0.035 Uiso 1 1 calc R . .
H8C H 0.4252 0.0836 0.1066 0.035 Uiso 1 1 calc R . .
C9 C 0.7561(2) 0.31569(12) 0.11525(7) 0.0189(5) Uani 1 1 d . . .
C10 C 0.7901(2) 0.34531(15) 0.06349(7) 0.0294(5) Uani 1 1 d . . .
H10A H 0.9013 0.3425 0.0614 0.044 Uiso 1 1 calc R . .
H10B H 0.7542 0.4049 0.0578 0.044 Uiso 1 1 calc R . .
H10C H 0.7363 0.3074 0.0383 0.044 Uiso 1 1 calc R . .
C11 C 0.8291(2) 0.22658(14) 0.12523(8) 0.0285(5) Uani 1 1 d . . .
H11A H 0.7820 0.1852 0.1007 0.043 Uiso 1 1 calc R . .
H11B H 0.8118 0.2074 0.1586 0.043 Uiso 1 1 calc R . .
H11C H 0.9401 0.2301 0.1228 0.043 Uiso 1 1 calc R . .
C12 C 0.8424(2) 0.37724(13) 0.15363(7) 0.0243(5) Uani 1 1 d . . .
H12A H 0.8268 0.3582 0.1871 0.036 Uiso 1 1 calc R . .
H12B H 0.8022 0.4361 0.1483 0.036 Uiso 1 1 calc R . .
H12C H 0.9527 0.3766 0.1498 0.036 Uiso 1 1 calc R . .
C13 C 0.3641(2) 0.10558(12) 0.25414(7) 0.0185(4) Uani 1 1 d . . .
H13B H 0.2935 0.1066 0.2230 0.022 Uiso 1 1 calc R . .
H13A H 0.3072 0.1252 0.2817 0.022 Uiso 1 1 calc R . .
C14 C 0.4296(2) 0.01607(12) 0.26417(7) 0.0205(5) Uani 1 1 d . . .
H14B H 0.3549 -0.0291 0.2515 0.025 Uiso 1 1 calc R . .
H14A H 0.4590 0.0068 0.3001 0.025 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 0.0000 0.0000 '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'
Mo Mo -1.6832 0.6857 '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'
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
O1 Mo1 O1 179.42(8) 2_655 . ?
O1 Mo1 O2 90.29(4) 2_655 . ?
O1 Mo1 O2 90.29(4) . . ?
O1 Mo1 Cl2 89.71(4) 2_655 . ?
O1 Mo1 Cl2 89.71(4) . . ?
O2 Mo1 Cl2 180.0 . . ?
O1 Mo1 Cl1 88.86(4) 2_655 . ?
O1 Mo1 Cl1 91.18(4) . . ?
O2 Mo1 Cl1 86.429(12) . . ?
Cl2 Mo1 Cl1 93.571(12) . . ?
O1 Mo1 Cl1 91.18(4) 2_655 2_655 ?
O1 Mo1 Cl1 88.85(4) . 2_655 ?
O2 Mo1 Cl1 86.431(12) . 2_655 ?
Cl2 Mo1 Cl1 93.569(12) . 2_655 ?
Cl1 Mo1 Cl1 172.86(2) . 2_655 ?
O1 Si1 C9 104.99(7) . . ?
O1 Si1 C5 104.40(7) . . ?
C9 Si1 C5 113.27(8) . . ?
O1 Si1 C1 108.26(8) . . ?
C9 Si1 C1 112.72(8) . . ?
C5 Si1 C1 112.43(9) . . ?
Si1 O1 Mo1 171.86(8) . . ?
C13 O2 C13 109.39(18) 2_655 . ?
C13 O2 Mo1 125.31(9) 2_655 . ?
C13 O2 Mo1 125.31(9) . . ?
C2 C1 C4 107.73(17) . . ?
C2 C1 C3 106.27(17) . . ?
C4 C1 C3 107.99(16) . . ?
C2 C1 Si1 112.62(14) . . ?
C4 C1 Si1 110.39(14) . . ?
C3 C1 Si1 111.61(13) . . ?
C8 C5 C6 105.39(16) . . ?
C8 C5 C7 108.01(16) . . ?
C6 C5 C7 108.44(16) . . ?
C8 C5 Si1 110.48(13) . . ?
C6 C5 Si1 112.32(14) . . ?
C7 C5 Si1 111.91(13) . . ?
C11 C9 C10 108.17(17) . . ?
C11 C9 C12 105.90(16) . . ?
C10 C9 C12 107.70(16) . . ?
C11 C9 Si1 111.63(13) . . ?
C10 C9 Si1 112.57(13) . . ?
C12 C9 Si1 110.57(13) . . ?
O2 C13 C14 104.61(14) . . ?
C13 C14 C14 102.67(12) . 2_655 ?
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
Mo1 O1 1.8348(12) 2_655 ?
Mo1 O1 1.8348(12) . ?
Mo1 O2 2.1676(17) . ?
Mo1 Cl2 2.3429(7) . ?
Mo1 Cl1 2.3689(5) . ?
Mo1 Cl1 2.3690(5) 2_655 ?
Si1 O1 1.7066(13) . ?
Si1 C9 1.9160(19) . ?
Si1 C5 1.923(2) . ?
Si1 C1 1.924(2) . ?
O2 C13 1.474(2) 2_655 ?
O2 C13 1.475(2) . ?
C1 C2 1.541(3) . ?
C1 C4 1.545(3) . ?
C1 C3 1.546(3) . ?
C5 C8 1.532(3) . ?
C5 C6 1.535(3) . ?
C5 C7 1.548(3) . ?
C9 C11 1.529(3) . ?
C9 C10 1.538(3) . ?
C9 C12 1.544(3) . ?
C13 C14 1.511(3) . ?
C14 C14 1.521(4) 2_655 ?
