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_4329177
_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            'C91 H89 B N2 O P4 W'
_chemical_formula_weight         1545.18
_chemical_name_common            W(CPh)(dppe)2(NCMe)+
_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                97.281(3)
_cell_angle_beta                 108.399(3)
_cell_angle_gamma                96.291(3)
_cell_formula_units_Z            2
_cell_length_a                   13.266(3)
_cell_length_b                   16.373(3)
_cell_length_c                   18.470(4)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      1.58
_cell_volume                     3728.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32909
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  0.8495
_exptl_absorpt_correction_T_min  0.6780
_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    1.377
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.104
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         17085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.3007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                16222
_reflns_number_total             17085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202622s_si_002_2.cif
_cod_data_source_block           ches19
_cod_original_cell_volume        3728.1(13)
_cod_database_code               4329177