Molybdenum and tungsten mono-isodiazene complexes with alkyl ligands as ring-opening metathesis polymerisation procatalysts. Crystal and molecular structures of [Mo(CH2CMe2Ph)3(NNPh2)(OC6F5)], [W(CH2SiMe3)3(NNPh2)(OC6F5)] and [WCl2(NNPh2)(OC6F5)2(thf )]
Dilworth, Jonathan R.; Gibson, Vernon C.; Redshaw, Carl; White, Andrew J. P.; Williams, David J.; Journal of the Chemical Society, Dalton Transactions  (1999) 2701–; doi:10.1039/a903770e

data_7027538
_publ_section_title
;
 Molybdenum and tungsten mono-isodiazene complexes with alkyl ligands as
 ring-opening metathesis polymerisation procatalysts. Crystal and
 molecular structures of [Mo(CH2CMe2Ph)3(NNPh2)(OC6F5)],
 [W(CH2SiMe3)3(NNPh2)(OC6F5)] and [WCl2(NNPh2)(OC6F5)2(thf&#x200A;)]
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2701
_journal_paper_doi               10.1039/a903770e
_journal_year                    1999
_chemical_formula_sum            'C30 H43 F5 N2 O Si3 W'
_chemical_formula_weight         810.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.841(7)
_cell_angle_beta                 90.338(8)
_cell_angle_gamma                110.944(8)
_cell_formula_units_Z            2
_cell_length_a                   9.9973(12)
_cell_length_b                   10.6644(8)
_cell_length_c                   18.1009(13)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      10.72
_cell_volume                     1802.0(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5686
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         2.44
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.334
_exptl_absorpt_correction_T_max  0.1596
_exptl_absorpt_correction_T_min  0.0477
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       'platy prisms'
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.704
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.00111(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_obs          0.0458
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+0.4424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1261
_refine_ls_wR_factor_obs         0.1173
_reflns_number_observed          4795
_reflns_number_total             5327
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903770esup1.cif
_cod_data_source_block           VG9759
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+0.4424P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+0.4424P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30 H43 N2 O F5 Si3 W'
_cod_database_code               7027538