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_4080389
_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         'C32 H40 N2 Ni2 O4 S2'
_chemical_formula_sum            'C32 H40 N2 Ni2 O4 S2'
_chemical_formula_weight         698.20
_chemical_name_systematic
;
 N,N'-bis(4-tolylsulfonyl)-
 4,9-diazadodeca-1,11-diene-6-yne-dinickel-cycloocta-1,4-diene
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                CHS-CD-137-00
_audit_creation_date             2012-08-15
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0276(14)
_cell_length_b                   16.379(2)
_cell_length_c                   17.013(2)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.9779
_cell_measurement_theta_min      2.2264
_cell_volume                     3072.9(7)
_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_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            118667
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         36.40
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  0.94863
_exptl_absorpt_correction_T_min  0.81013
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.640
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         14840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0379P)^2^+4.9419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                13946
_reflns_number_total             14840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301160m_si_002.cif
_cod_data_source_block           4
_cod_original_sg_symbol_Hall     'p 2ac 2ab'
_cod_original_sg_symbol_H-M      'p 21 21 21'
_cod_database_code               4080389