Nickel(0) Complexes of Acyclic Polyunsaturated Aza Ligands
Brun, Sandra; Torres, Óscar; Pla-Quintana, Anna; Roglans, Anna; Goddard, Richard; Pörschke, Klaus-Richard; Organometallics 32 (2013) 1710–; doi:10.1021/om301160m

data_4080390
_publ_section_title
;
 Nickel(0) Complexes of Acyclic Polyunsaturated Aza Ligands
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1710
_journal_paper_doi               10.1021/om301160m
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        tetrahydrofuran
_chemical_formula_moiety         '2(C25 H32 N2 Ni O4 S2), C4 H8 O'
_chemical_formula_sum            'C54 H72 N4 Ni2 O9 S4'
_chemical_formula_weight         1166.82
_chemical_name_systematic
;
 N,N'-bis(4-tolylsulfonyl)-
 4,9-diazatrideca-1,6-diene-11-yne-nickel hemi-tetrahydrofuran solute
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                BMW-BB-238-01
_audit_creation_date             2011-10-25
_cell_angle_alpha                90.00
_cell_angle_beta                 105.413(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7565(18)
_cell_length_b                   15.921(3)
_cell_length_c                   16.427(3)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.4109
_cell_measurement_theta_min      2.3439
_cell_volume                     2712.0(8)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (G. M. Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0130
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            103280
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         36.51
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.92264
_exptl_absorpt_correction_T_min  0.84663
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.095
_refine_diff_density_max         3.688
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         13159
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0686P)^2^+2.8405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                11646
_reflns_number_total             13159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301160m_si_002.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4080390