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_7027537
_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            'C48 H49 F5 Mo N2 O'
_chemical_formula_weight         860.83
_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                87.302(12)
_cell_angle_beta                 81.012(15)
_cell_angle_gamma                66.879(11)
_cell_formula_units_Z            2
_cell_length_a                   11.809(3)
_cell_length_b                   11.9047(14)
_cell_length_c                   16.348(3)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.77
_cell_volume                     2087.4(7)
_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      203(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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6898
_diffrn_reflns_theta_max         61.99
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        6.74
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.074
_exptl_absorpt_correction_T_max  0.8012
_exptl_absorpt_correction_T_min  0.2891
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       Prismatic_plates
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.908
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0013(2)
_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   1.022
_refine_ls_goodness_of_fit_obs   1.028
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.058
_refine_ls_restrained_S_obs      1.028
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_obs          0.0408
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+1.9378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2221
_refine_ls_wR_factor_obs         0.1100
_reflns_number_observed          6227
_reflns_number_total             6537
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903770esup1.cif
_cod_data_source_block           VG9713
_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^)+(0.0664P)^2^+1.9378P] 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^)+(0.0664P)^2^+1.9378P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2087.5(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C48 H49 N2 O F5 Mo'
_cod_database_code               7027537