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_1514529
_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         'C27 H21 B0.50 Ni F11 P1.5'
_chemical_formula_sum            'C33 H30.5 B0.5 F11 N7 Ni O0.5 P1.5'
_chemical_formula_weight         852.71
_chemical_name_common            '[Ni(bpy2py)(CH3CN)]*1.5PF6*0.5BF4*Et2O'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.443(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.605(3)
_cell_length_b                   26.456(6)
_cell_length_c                   12.584(3)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.4128
_cell_measurement_theta_min      2.3518
_cell_volume                     3517.3(15)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38001
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.9253
_exptl_absorpt_correction_T_min  0.8467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1734
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.663
_refine_diff_density_min         -1.717
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         6459
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0736P)^2^+9.2270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                5933
_reflns_number_total             6459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc51660a.txt
_cod_data_source_block           3
_cod_original_cell_volume        3517.3(14)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C33 H30.50 B0.50 F11 N7 Ni O0.50 P1.50'
_cod_database_code               1514529