Dihydrogen activation by a tungsten-alkylidyne complex: toward photoredox chromophores that deliver renewable reducing equivalents
Cesar A. Morales-Verdejo; Michael I. Newsom; Brian W. Cohen; Hunter B. Vibbert; Michael D. Hopkins; Chem.Commun. 49 (2013) 10566–; doi:10.1039/c3cc45606d

data_7110002
_publ_section_title
;
 Dihydrogen activation by a tungsten-alkylidyne complex: toward photoredox
 chromophores that deliver renewable reducing equivalents
;
_journal_name_full               Chem.Commun.
_journal_page_first              10566
_journal_paper_doi               10.1039/c3cc45606d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C66 H61 Cl F6 P5 W'
_chemical_formula_weight         1342.30
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_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                78.017(4)
_cell_angle_beta                 79.887(4)
_cell_angle_gamma                80.575(4)
_cell_formula_units_Z            2
_cell_length_a                   11.066(3)
_cell_length_b                   12.217(3)
_cell_length_c                   22.205(6)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.72
_cell_volume                     2865.6(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 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33829
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    2.264
_exptl_absorpt_correction_T_max  0.8053
_exptl_absorpt_correction_T_min  0.6602
_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    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1354
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.198
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         13542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                11867
_reflns_number_total             13542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45606d.txt
_cod_data_source_block           brian02s
_cod_original_cell_volume        2865.5(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110002