Nickel(0) Complexes of Polyunsaturated Azamacrocyclic Ligands
Brun, Sandra; Pla-Quintana, Anna; Roglans, Anna; Pörschke, Klaus-Richard; Goddard, Richard; Organometallics 31 (2012) 1983–; doi:10.1021/om201271y

data_4076503
_publ_section_title
;
 Nickel(0) Complexes of Polyunsaturated Azamacrocyclic Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1983
_journal_paper_doi               10.1021/om201271y
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        tetrahydrofuran
_chemical_formula_moiety         'C39.67 H47 N3 Ni1.83 O6 S3'
_chemical_formula_sum            'C39.67 H47 N3 Ni1.83 O6 S3'
_chemical_formula_weight         865.77
_chemical_name_systematic
;
 (E,E)-1,6,11-tris(4-tolylsulfonyl)-1,6,11-triazacyclopentadeca-3,8-diene-
 13-yne-nickel(0)-1,5-cyclooctadiene-nickel(0)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                CHS-CD-138-00
_audit_creation_date             2011-10-14
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.539(3)
_cell_length_b                   18.881(3)
_cell_length_c                   11.2747(15)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.8732
_cell_measurement_theta_min      2.1971
_cell_volume                     3946.5(10)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1310
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            110518
_diffrn_reflns_theta_full        31.45
_diffrn_reflns_theta_max         31.45
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_T_max  0.96150
_exptl_absorpt_correction_T_min  0.82857
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             1814
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         6679
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+38.4966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.2199
_reflns_number_gt                4745
_reflns_number_total             6679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201271y_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        3946.6(9)
_cod_database_code               4076503