X-ray Crystallographic, Multifrequency Electron Paramagnetic Resonance, and Density Functional Theory Characterization of the Ni(P(Cy)2N(tBu)2)2(n+) Hydrogen Oxidation Catalyst in the Ni(I) Oxidation State.
Niklas, Jens; Westwood, Mark; Mardis, Kristy L.; Brown, Tiara L.; Pitts-McCoy, Anthony M; Hopkins, Michael D.; Poluektov, Oleg G.; Inorganic chemistry 54 (2015) 6226–6234; doi:10.1021/acs.inorgchem.5b00445

data_4343388
_publ_section_title
;
 X-ray Crystallographic, Multifrequency Electron Paramagnetic Resonance,
 and Density Functional Theory Characterization of the
 Ni(P(Cy)2N(tBu)2)2(n+) Hydrogen Oxidation Catalyst in the Ni(I) Oxidation
 State.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6226
_journal_page_last               6234
_journal_paper_doi               10.1021/acs.inorgchem.5b00445
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C48 H96 N4 Ni P4, B F4'
_chemical_formula_sum            'C48 H96 B F4 N4 Ni P4'
_chemical_formula_weight         998.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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
;
dual-space method as implemented in SHELXT
;
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.225(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.729(6)
_cell_length_b                   11.661(3)
_cell_length_c                   20.503(6)
_cell_measurement_reflns_used    9611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.65
_cell_measurement_theta_min      2.33
_cell_volume                     5268(2)
_computing_cell_refinement       'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 v.2014.9-0 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_molecular_graphics
;
Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst (1997), 30, 565

Mercury: visualization and analysis of crystal structures
C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, 
R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006 
;
_computing_publication_material  'APEX2 v.2014.9-0 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_source         'INCOATEC ImuS micro-focus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            87240
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.134
_diffrn_reflns_theta_max         25.134
_diffrn_reflns_theta_min         1.976
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (version 2012/4) as implemented in APEX2, version 2014.9-0, Bruker AXS
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.920
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+5.3572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3745
_reflns_number_total             4694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00445_si_002.cif
_cod_data_source_block           west01
_cod_depositor_comments          'Adding full bibliography for 4343388.cif.'
_cod_database_code               4343388
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.636
_shelx_estimated_absorpt_t_max   0.886
_shelx_res_checksum              55642
_shelx_hkl_checksum              99540