Hydrogen production from water using a bis(imino)pyridine molybdenum electrocatalyst.
Pal, Raja; Laureanti, Joseph A.; Groy, Thomas L.; Jones, Anne K.; Trovitch, Ryan J.; Chemical communications (Cambridge, England) 52 (2016) 11555–11558; doi:10.1039/c6cc04946j

data_7124837
_publ_section_title
;
 Hydrogen production from water using a bis(imino)pyridine molybdenum
 electrocatalyst.
;
_journal_issue                   77
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11555
_journal_page_last               11558
_journal_paper_doi               10.1039/c6cc04946j
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
;
C39 H41 Mo N3 O P2, 2(F6 P), 1.745(C3 H6 O), 0.255(C3 O)
;
_chemical_formula_sum            'C45 H51.47 F12 Mo N3 O3 P4'
_chemical_formula_weight         1130.18
_chemical_name_common            PF6PDIMoO
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-08-10 deposited with the CCDC.
2016-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3031(6)
_cell_length_b                   15.9629(6)
_cell_length_c                   20.6295(8)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    123.(2)
_cell_measurement_theta_max      25.0008
_cell_measurement_theta_min      2.2951
_cell_volume                     4876.2(3)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2015.5.1.3'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123.(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2 Diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38574
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.88
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'parallelapipedal block'
_exptl_crystal_F_000             2306
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.113
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.644
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8623
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+1.5679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1233
_reflns_number_gt                7313
_reflns_number_total             8623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04946j2.cif
_cod_data_source_block           PF6PDIMoO
_cod_database_code               7124837
_shelx_res_checksum              63780