Synthesis, spectroscopy and electronic structure of the vinylidene and alkynyl complexes [W(C=CHR)(dppe)(η-C₇H₇)](+) and [W(C≡CR)(dppe)(η-C₇H₇](n+) (n = 0 or 1).
Lancashire, Hannah N.; Brown, Neil J.; Carthy, Laura; Collison, David; Fitzgerald, Emma C.; Edge, Ruth; Helliwell, Madeleine; Holden, Mark; Low, Paul J.; McDouall, Joseph J. W.; Whiteley, Mark W.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 1267–1278; doi:10.1039/c0dt01150a

data_7014783
_publ_section_title
;
 Synthesis, spectroscopy and electronic structure of the vinylidene and
 alkynyl complexes [W(C=CHR)(dppe)(\h-C&#x2087;H&#x2087;)](+) and
 [W(C\\tb CR)(dppe)(\h-C&#x2087;H&#x2087;](n+) (n = 0 or 1).
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1267
_journal_page_last               1278
_journal_paper_doi               10.1039/c0dt01150a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C33 H31 Br P2 W; CH2Cl2'
_chemical_formula_sum            'C34 H33 Br Cl2 P2 W'
_chemical_formula_weight         838.20
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.3121(10)
_cell_length_b                   9.3925(4)
_cell_length_c                   27.8933(15)
_cell_measurement_reflns_used    14872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6167
_cell_measurement_theta_min      2.7109
_cell_volume                     6107.5(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Oxford Diffraction XCalibur 2'
_diffrn_measurement_method       'phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            44231
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    5.395
_exptl_absorpt_correction_T_max  0.4117
_exptl_absorpt_correction_T_min  0.2215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.345
_refine_diff_density_min         -5.933
_refine_diff_density_rms         0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7189
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1211P)^2^+137.8089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2154
_refine_ls_wR_factor_ref         0.2322
_reflns_number_gt                4653
_reflns_number_total             7189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01150A.TXT
_cod_data_source_block           omww34
_cod_original_sg_symbol_H-M      pcab
_cod_database_code               7014783