Catalytic proton reduction with transition metal complexes of the redox-active ligand bpy2PYMe
Nippe, Michael; Khnayzer, Rony S.; Panetier, Julien A.; Zee, David Z.; Olaiya, Babatunde S.; Head-Gordon, Martin; Chang, Christopher J.; Castellano, Felix N.; Long, Jeffrey R.; Chemical Science 4 (2013) 3934–; doi:10.1039/c3sc51660a

data_1514531
_publ_section_title
;
 Catalytic proton reduction with transition metal complexes of the
 redox-active ligand bpy2PYMe
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3934
_journal_paper_doi               10.1039/c3sc51660a
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C29 H21 Zn F6 N5 O6 S2'
_chemical_formula_sum            'C31 H24 F6 N6 O6 S2 Zn'
_chemical_formula_weight         820.05
_chemical_name_common            '[Zn(bpy2py)OTf)OTf*CH3CN'
_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                92.8740(10)
_cell_angle_beta                 91.8050(10)
_cell_angle_gamma                91.2320(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8290(3)
_cell_length_b                   12.2969(3)
_cell_length_c                   13.4196(4)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3584
_cell_measurement_theta_min      2.1923
_cell_volume                     1618.70(8)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25512
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  0.8592
_exptl_absorpt_correction_T_min  0.7646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         5878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0387P)^2^+1.6198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                5558
_reflns_number_total             5878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc51660a.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1514531