Synthesis and crystal structure of the 16 e− cationic tungsten(IV) complex [WCp*(4,4′-Me2bipy)Cl2]+BPh4− †
Cremer, Christian; Burger, Peter; Journal of the Chemical Society, Dalton Transactions  (1999) 1967–; doi:10.1039/a902743b

data_7027439
_publ_section_title
;
 Synthesis and crystal structure of the 16 e&#x2212; cationic tungsten(IV)
 complex [WCp*(4,4&#x2032;-Me2bipy)Cl2]+BPh4&#x2212;&#x200A;&#x2020;
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1967
_journal_paper_doi               10.1039/a902743b
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_structural     'Cp*W(Me-bipy)(CO)Cl2+ BPh4- * C2H4Cl2'
_chemical_formula_sum            'C49 H51 B Cl4 N2 O W'
_chemical_formula_weight         1020.38
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 115.132(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.428(2)
_cell_length_b                   9.2642(6)
_cell_length_c                   23.646(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    183(2)
_cell_volume                     4448.0(7)
_computing_cell_refinement       'STOE IPDS PROGRAM PACKAGE'
_computing_data_collection       'STOE IPDS PROGRAM PACKAGE'
_computing_data_reduction        'STOE IPDS PROGRAM PACKAGE'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1998)'
_computing_publication_material  'SHELXL-93,  Platon (Spek, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1988)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'STOE IPDS'
_diffrn_measurement_method       'Image Plate'
_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    0.0432
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8462
_diffrn_reflns_theta_max         25.89
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/a
_exptl_crystal_description       'rect. parallelepiped'
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.971
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       n/a
_refine_ls_extinction_method     n/a
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_obs          0.0280
_refine_ls_shift/esd_max         -0.657
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0770
_refine_ls_wR_factor_obs         0.0668
_reflns_number_observed          6344
_reflns_number_total             8462
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902743bsup1.cif
_cod_data_source_block           4_Me+BPh4-
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'n/a' was changed to '?' - the value
is undefined or not given.

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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^)+(0.0404P)^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^)+(0.0404P)^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        4448.0(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027439