Hydrogen production using cobalt-based molecular catalysts containing a proton relay in the second coordination sphere
Jacobsen, George M.; Yang, Jenny Y.; Twamley, Brendan; Wilson, Aaron D.; Bullock, R. Morris; Rakowski DuBois, M.; DuBois, Daniel L.; Energy & Environmental Science 1 (2008) 167–; doi:10.1039/b805309j

data_1515997
_publ_section_title
;
 Hydrogen production using cobalt-based molecular catalysts containing a
 proton relay in the second coordination sphere
;
_journal_issue                   1
_journal_name_full               'Energy &amp; Environmental Science'
_journal_page_first              167
_journal_paper_doi               10.1039/b805309j
_journal_volume                  1
_journal_year                    2008
_chemical_formula_moiety         'C56 H56 Cl Co N4 P4, 0.5(B F4), 0.5(B F4)'
_chemical_formula_sum            'C56 H56 B Cl Co F4 N4 P4'
_chemical_formula_weight         1090.12
_chemical_name_common            '[RCoCl][BF4]'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 121.872(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.2939(13)
_cell_length_b                   12.9425(5)
_cell_length_c                   28.6361(11)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.38
_cell_volume                     10793.8(7)
_computing_cell_refinement       'SAINT+ v. 7.23a (Bruker, 2006)'
_computing_data_collection       'SMART v. 5.632 (Bruker, 2006)'
_computing_data_reduction        'SAINT+ v. 7.23a (Bruker, 2006)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)'
_computing_structure_refinement  'XL, SHELXTL v. 6.14 (Bruker, 2003)'
_computing_structure_solution    'XS, SHELXTL v. 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            62971
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.40
_diffrn_source                   'normal-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.9529
_exptl_absorpt_correction_T_min  0.7851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2007/4 (Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             4520
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.597
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         9775
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+14.8951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                7862
_reflns_number_total             9775
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b805309j.txt
_cod_data_source_block           bt1161
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1515997