Synthesis, Characterization, and Catalytic Activity of Nickel(II) Alkyl Complexes Supported by Pyrrole‒Diphosphine Ligands
Venkanna, Gopaladasu T.; Tammineni, Swetha; Arman, Hadi D.; Tonzetich, Zachary J.; Organometallics 32 (2013) 4656–; doi:10.1021/om400630q

data_4081355
_publ_section_title
;
 Synthesis, Characterization, and Catalytic Activity of Nickel(II) Alkyl
 Complexes Supported by Pyrrole--Diphosphine Ligands
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4656
_journal_paper_doi               10.1021/om400630q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C32 H31 N Ni P2, 0.5(C6 H6)'
_chemical_formula_sum            'C35 H34 N Ni P2'
_chemical_formula_weight         589.27
_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                99.531(2)
_cell_angle_beta                 90.6768(12)
_cell_angle_gamma                109.668(3)
_cell_formula_units_Z            4
_cell_length_a                   10.7014(14)
_cell_length_b                   14.3790(19)
_cell_length_c                   20.688(3)
_cell_measurement_reflns_used    14533
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      2.0
_cell_volume                     2948.4(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17086
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         11533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                10484
_reflns_number_total             11533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400630q_si_002.cif
_cod_data_source_block           '[Ni(C2H5)(PNP-Ph)]_-_7'
_cod_depositor_comments
;

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1175.34
_cod_original_formula_moiety       'C32 H27.80 N Ni P2, C32 H31 N Ni P2, C6 H6'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C70 H64.80 N2 Ni2 P4'
_cod_database_code               4081355