A Diphenylcyclopropene Complex of Tungsten, [WCl~2~O(PMePh~2~)~2~(η^2^-3,3-diphenylcyclopropene)], Precursor to a Tungsten‒Oxo‒Olefin Metathesis Catalyst
Day, M. W.; Wilhelm, T. E.; Grubbs, R. H.; Acta Crystallographica Section C 52 (1996) 2460–2462; doi:10.1107/S0108270196006464

data_2005471
_publ_section_title
;
 A Diphenylcyclopropene Complex of Tungsten,
 [WCl~2~O(PMePh~2~)~2~(\h^2^-3,3-diphenylcyclopropene)], Precursor to a
 Tungsten--Oxo--Olefin Metathesis Catalyst
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2460
_journal_page_last               2462
_journal_paper_doi               10.1107/S0108270196006464
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[W Cl2 O (C15 H12) (C13 H13 P)2]'
_chemical_formula_sum            'C41 H38 Cl2 O P2 W'
_chemical_formula_weight         863.40
_chemical_name_systematic
;
 Dichloro-bis(diphenylmethylphosphine)-
(\h^2^-3,3-diphenylcyclopropene)-oxo-tungsten
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.494(8)
_cell_length_b                   9.857(3)
_cell_length_c                   20.886(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.3
_cell_measurement_theta_min      9.5
_cell_volume                     3740(2)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CRYM (Duchamp, 1964)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD-4
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11266
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        'within counting statistics'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.35
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   '\y scan (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       'thick needles'
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.38
_refine_diff_density_min         -0.73
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.502
_refine_ls_goodness_of_fit_obs   1.47
_refine_ls_hydrogen_treatment    'Hydrogens refined as riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         4831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.549
_refine_ls_restrained_S_obs      1.468
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_obs          0.036
_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^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0765
_refine_ls_wR_factor_obs         0.062
_reflns_number_observed          3671
_reflns_number_total             4881
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bk1246.cif
_cod_data_source_block           TEW1
_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 

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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w = 1/\s^2^(Fo^2^)' 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^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3739(2)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2005471