Ground-State and Excited-State Structures of Tungsten-Benzylidyne Complexes
Benjamin M. Lovaasen; Jenny V. Lockard; Brian W. Cohen; Shujiang Yang; Xiaoyi Zhang; Cheslan K. Simpson; Lin X. Chen; Michael D. Hopkins; Inorganic Chemistry 51 (2012) 5660–5670; doi:10.1021/ic202622s

data_4329176
_publ_section_title
;
 Ground-State and Excited-State Structures of Tungsten-Benzylidyne
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5660
_journal_page_last               5670
_journal_paper_doi               10.1021/ic202622s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C61 H54.5 Cl2.5 F3 O3 P4 S W'
_chemical_formula_weight         1320.96
_chemical_name_common            W(CPh)(dppe)2Cl+
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.834(5)
_cell_angle_beta                 90.439(5)
_cell_angle_gamma                97.102(5)
_cell_formula_units_Z            2
_cell_length_a                   11.195(3)
_cell_length_b                   12.247(3)
_cell_length_c                   22.433(6)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.72
_cell_volume                     2973.9(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0956
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21751
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    2.250
_exptl_absorpt_correction_T_max  0.9356
_exptl_absorpt_correction_T_min  0.8063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption corrections were made based on correspondance of
equivalent intensities usingprogram SADABS (G. Sheldrick, Bruker 
Analytical X-ray Systems, Madison, WI)
;
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.127
_refine_diff_density_min         -2.509
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                8795
_reflns_number_total             10454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202622s_si_002_1.cif
_cod_data_source_block           brian07s
_cod_original_formula_sum        'C61 H54.50 Cl2.50 F3 O3 P4 S W'
_cod_database_code               4329176