Four-Coordinate Mo(II) as (silox)2Mo(PMe3)2 and Its W(IV) Congener (silox)2HW(η2-CH2PMe2)(PMe3) (silox =tBu3SiO)
David S. Kuiper; Peter T. Wolczanski; Emil B. Lobkovsky; Thomas R. Cundari; Inorganic Chemistry 47 (2008) 10542–10553; doi:10.1021/ic8011958

data_4306347
_publ_section_title
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Four-Coordinate Mo(II) as (silox)2Mo(PMe3)2 and Its W(IV) Congener
(silox)2HW(\h2-CH2PMe2)(PMe3) (silox =tBu3SiO)
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_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         'C30 H72 Mo O2 P2 Si2'
_chemical_formula_sum            'C30 H72 Mo O2 P2 Si2'
_chemical_formula_weight         678.94
_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                 90.252(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2725(4)
_cell_length_b                   28.0138(13)
_cell_length_c                   15.0447(7)
_cell_measurement_reflns_used    3529
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.19
_cell_measurement_theta_min      2.58
_cell_volume                     3907.9(3)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0728
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25756
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.9876
_exptl_absorpt_correction_T_min  0.9064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green-red
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+16.2911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                3529
_reflns_number_total             4052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8011958_si_001_4.cif
_cod_data_source_block           dk18
_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 
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_cod_database_code               4306347