Stabilization of Nickel Complexes with Ni0···H‒N Bonding Interactions Using Sterically Demanding Cyclic Diphosphine Ligands
Wiedner, Eric S.; Yang, Jenny Y.; Chen, Shentan; Raugei, Simone; Dougherty, William G.; Kassel, W. Scott; Helm, Monte L.; Bullock, R. Morris; Rakowski DuBois, M.; DuBois, Daniel L.; Organometallics 31 (2012) 144–; doi:10.1021/om200709z

data_4067813
_publ_section_title
;
 Stabilization of Nickel Complexes with Ni0&#x00B7;&#x00B7;&#x00B7;H--N
 Bonding Interactions Using Sterically Demanding Cyclic Diphosphine
 Ligands
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              144
_journal_paper_doi               10.1021/om200709z
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C52 H80 N4 Ni P4, 2(C2 H3 N), B F4'
_chemical_formula_sum            'C56 H86 B F4 N6 Ni P4'
_chemical_formula_weight         1112.71
_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                86.220(3)
_cell_angle_beta                 70.099(3)
_cell_angle_gamma                77.714(3)
_cell_formula_units_Z            2
_cell_length_a                   13.4155(15)
_cell_length_b                   13.7624(15)
_cell_length_c                   19.175(2)
_cell_measurement_reflns_used    9029
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.26
_cell_volume                     3252.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58463
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.9738
_exptl_absorpt_correction_T_min  0.9262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1186
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.548
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         11914
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0942
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1741P)^2^+15.7368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2735
_refine_ls_wR_factor_ref         0.2999
_reflns_number_gt                8827
_reflns_number_total             11914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200709z_si_002.cif
_cod_data_source_block           reint
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3252.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4067813