WCl(η2-C2Ph2)(η6-C6Ph6H): A Compound Containing a Metallacycloheptatriene Unit from Trimerization of Diphenylacetylene with W(NMe3)(η2-C2Ph2)3
Yeh, Wen-Yann; Peng, Shie-Ming; Lee, Gene-Hsiang; Organometallics 21 (2002) 3058–; doi:10.1021/om0201009

data_4076831
_publ_section_title
;
 WCl(\h2-C2Ph2)(\h6-C6Ph6H):&#x00A0; A Compound Containing a
 Metallacycloheptatriene Unit from Trimerization of Diphenylacetylene with
 W(NMe3)(\h2-C2Ph2)3
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3058
_journal_paper_doi               10.1021/om0201009
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C56 H42 Cl W'
_chemical_formula_weight         934.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 98.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.286(3)
_cell_length_b                   15.150(3)
_cell_length_c                   21.303(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
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_cell_measurement_theta_min      7.29
_cell_volume                     4239.7(15)
_computing_cell_refinement       'NONIUS CAD4'
_computing_data_collection       'NONIUS CAD4'
_computing_data_reduction        'NRCSDP DATRD2'
_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      295(2)
_diffrn_measurement_device       'NONIUS CAD4'
_diffrn_measurement_method       '\w--2\q 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.826
_exptl_absorpt_correction_T_max  0.5300
_exptl_absorpt_correction_T_min  0.4278
_exptl_absorpt_correction_type   'empirical used psi-scan'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.40
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_refine_diff_density_max         1.346
_refine_diff_density_min         -0.870
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6195
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_obs          0.0313
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0797
_refine_ls_wR_factor_obs         0.0751
_reflns_number_observed          5157
_reflns_number_total             6195
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om0201009.cif
_cod_data_source_block           ic7053
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0427P)^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^)+(0.0427P)^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_cell_volume        4239.6(15)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4076831