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_7027438
_publ_section_title
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 Synthesis and crystal structure of the 16 e&#x2212; cationic tungsten(IV)
 complex [WCp*(4,4&#x2032;-Me2bipy)Cl2]+BPh4&#x2212;&#x200A;&#x2020;
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_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)Cl2+BPh4-
_chemical_formula_sum            'C46 H47 B Cl2 N2 W'
_chemical_formula_weight         893.42
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6720(10)
_cell_length_b                   16.362(2)
_cell_length_c                   21.122(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    193(2)
_cell_volume                     3977.2(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    'Platon (Spek, 1997)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993);'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1988)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'STOE IPDS Image Plate system'
_diffrn_measurement_method       'Image Plate with incremental Phi-angle'
_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    0.0409
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7678
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    3.074
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/a
_exptl_crystal_description       'rectangular parallelepiped'
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       n/a
_refine_ls_extinction_method     n/a
_refine_ls_goodness_of_fit_all   0.991
_refine_ls_goodness_of_fit_obs   1.135
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_restrained_S_obs      1.135
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_obs          0.0192
_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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0372
_refine_ls_wR_factor_obs         0.0363
_reflns_number_observed          5722
_reflns_number_total             7678
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902743bsup1.cif
_cod_data_source_block           complex_2Me+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^)+(0.0100P)^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^)+(0.0100P)^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      P2(1)/c
_cod_database_code               7027438