Generation of Powerful Tungsten Reductants by Visible Light Excitation
Wesley Sattler; Maraia E. Ener; James D. Blakemore; Aaron A. Rachford; Paul J. LaBeaume; James W. Thackeray; James F. Cameron; Jay R. Winkler; Harry B. Gray; Journal of the American Chemical Society 135 (2013) 10614–10617; doi:10.1021/ja4047119

data_4120151
_publ_section_title
;
 Generation of Powerful Tungsten Reductants by Visible Light Excitation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10614
_journal_page_last               10617
_journal_paper_doi               10.1021/ja4047119
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C90 H114 N6 W'
_chemical_formula_weight         1463.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                69.655(3)
_cell_angle_beta                 72.573(3)
_cell_angle_gamma                69.561(3)
_cell_formula_units_Z            1
_cell_length_a                   13.1880(6)
_cell_length_b                   13.2245(6)
_cell_length_c                   13.4292(6)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.26
_cell_measurement_theta_min      2.59
_cell_volume                     2015.04(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54470
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  0.9035
_exptl_absorpt_correction_T_min  0.4072
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             770
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.07
_refine_diff_density_max         5.952
_refine_diff_density_min         -2.338
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         12187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0844P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1196
_reflns_number_gt                12024
_reflns_number_total             12187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4047119_si_002.cif
_cod_data_source_block           ws10
_cod_original_cell_volume        2015.04(16)
_cod_database_code               4120151