A tungsten complex containing a highly delocalized metal‒ligand system
Colquhoun, Howard M.; Chippindale, Ann M.; Chan, Yun Fu; Acta Crystallographica Section C 64 (2008) m390–m393; doi:10.1107/S0108270108037232

data_2016886
_publ_section_title
;
 A tungsten complex containing a highly delocalized metal--ligand
 system
;
_journal_coeditor_code           SQ3171
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m390
_journal_page_last               m393
_journal_paper_doi               10.1107/S0108270108037232
_journal_volume                  64
_journal_year                    2008
_chemical_formula_moiety         'C76 H66 Br Cl N2 P5 W, F6 P, 0.6(C H2 Cl2)'
_chemical_formula_sum            'C76.6 H67.2 Br Cl2.2 F6 N2 P6 W'
_chemical_formula_weight         1657.27
_chemical_name_systematic
;
Bis[1,2-(diphenylphosphino)ethane]bromido{chloro[3-
(triphenylphosphonio)cyclopentadienylidene]diazomethanediido}tungsten(IV)
hexafluorophosphate dichloromethane 0.6-solvate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 98.236(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2621(10)
_cell_length_b                   14.7060(10)
_cell_length_c                   28.934(2)
_cell_measurement_reflns_used    16178
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     7690.4(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>,  1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17372
_diffrn_reflns_theta_full        25.832
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         5.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.279
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.01
_refine_diff_density_min         -0.70
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0868
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     875
_refine_ls_number_reflns         9841
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.003205
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 0.292 0.504E-01 0.896E-01
Watkin, D. (1994). <i>Acta Cryst.</i> A<b>50</b>, 411--437.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0796
_refine_ls_wR_factor_gt          0.0369
_refine_ls_wR_factor_ref         0.0369
_reflns_number_gt                9841
_reflns_number_total             17372
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            sq3171.cif
_cod_data_source_block           II
_cod_original_cell_volume        7690.3(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016886
_cod_database_fobs_code          2016886