Light-driven hydrogen evolution with a nickel thiosemicarbazone redox catalyst featuring Ni⋯H interactions under basic conditions
Jing, Xu; Wu, Pengyan; Liu, Xin; Yang, Linlin; He, Cheng; Duan, Chunying; New J. Chem. 39 (2015) 1051–; doi:10.1039/C4NJ01540A

data_7054570
_publ_section_title
;
 Light-driven hydrogen evolution with a nickel thiosemicarbazone redox
 catalyst featuring Ni&#x22EF;H interactions under basic conditions
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1051
_journal_paper_doi               10.1039/C4NJ01540A
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C42 H47 B F4 N6 Ni O5 P2 S2'
_chemical_formula_weight         987.44
_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                93.409(6)
_cell_angle_beta                 91.482(6)
_cell_angle_gamma                111.218(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4300(8)
_cell_length_b                   12.8553(10)
_cell_length_c                   21.7668(18)
_cell_measurement_reflns_used    3451
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.32
_cell_volume                     2452.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17600
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         8612
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2148
_reflns_number_gt                6196
_reflns_number_total             8612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj01540a2.cif
_cod_data_source_block           sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 7054569--7054570.cif.
;
_cod_original_cell_volume        2452.3(3)
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7054570