Study of an S = 1 Ni(II) pincer electrocatalyst precursor for aqueous hydrogen production based on paramagnetic 1H NMR.
Luca, Oana R.; Konezny, Steven J.; Paulson, Eric K.; Habib, Fatemah; Luthy, Kurt M.; Murugesu, Muralee; Crabtree, Robert H.; Batista, Victor S.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8802–8807; doi:10.1039/c3dt50528f

data_7023020
_publ_section_title
;
 Study of an S = 1 Ni(II) pincer electrocatalyst precursor for aqueous
 hydrogen production based on paramagnetic 1H NMR.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8802
_journal_page_last               8807
_journal_paper_doi               10.1039/c3dt50528f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C26.62 H29.62 Br2 Cl0.77 N3.62 Zn'
_chemical_formula_weight         652.77
_chemical_name_systematic
;
?
;
_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                 107.768(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0658(2)
_cell_length_b                   14.9486(3)
_cell_length_c                   14.4262(10)
_cell_measurement_reflns_used    12121
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      65.1
_cell_measurement_theta_min      6.9
_cell_volume                     2683.3(2)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_molecular_graphics
;
'ORTEP-3 (Farrugia, 1997)'
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12805
_diffrn_reflns_theta_full        65.06
_diffrn_reflns_theta_max         65.06
_diffrn_reflns_theta_min         6.91
_exptl_absorpt_coefficient_mu    5.625
_exptl_absorpt_correction_T_max  0.8063
_exptl_absorpt_correction_T_min  0.6031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1311
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4435
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0536P)^2^+5.9705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                4090
_reflns_number_total             4435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50528f.cif
_cod_data_source_block           kl01
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7023020