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_7027539
_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            'C28 H18 Cl2 F10 N2 O3 W'
_chemical_formula_weight         875.19
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.29(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.908(2)
_cell_length_b                   13.007(2)
_cell_length_c                   21.660(4)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.54
_cell_measurement_theta_min      5.38
_cell_volume                     3041.0(9)
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            2551
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        6.13
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.8154
_exptl_absorpt_correction_T_min  0.3887
_exptl_absorpt_correction_type   Lamina
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       'platy prisms'
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_obs          0.0360
_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^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0858
_refine_ls_wR_factor_obs         0.0803
_reflns_number_observed          2050
_reflns_number_total             2412
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903770esup1.cif
_cod_data_source_block           VG9760
_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 2.4.2 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^)+(0.0421P)^2^+0.0000P] 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^)+(0.0421P)^2^+0.0000P] 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      C2/c
_cod_original_formula_sum        'C28 H18 N2 O3 F10 Cl2 W'
_cod_database_code               7027539