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_4076502
_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         'C33 H37 N3 Ni O6 S3, 5(C4 H8 O)'
_chemical_formula_sum            'C53 H77 N3 Ni O11 S3'
_chemical_formula_weight         1087.07
_chemical_name_systematic
;
 (E,E)-1,6,11-tris(4-tolylsulfonyl)-1,6,11-triazacyclopentadeca-3,8-diene-
 13-ynenickel(0)-1,5-cyclooctadiene-nickel(0) penta-tetrahydrofuran solute
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                CHS-CD-112-10
_audit_creation_date             2011-12-13
_cell_angle_alpha                90.00
_cell_angle_beta                 112.408(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.5404(14)
_cell_length_b                   17.8908(14)
_cell_length_c                   13.864(3)
_cell_measurement_reflns_used    40133
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.9999
_cell_measurement_theta_min      2.7786
_cell_volume                     2646.3(7)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37802
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.92393
_exptl_absorpt_correction_T_min  0.88050
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       prism
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         7920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0576P)^2^+6.8832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1810
_reflns_number_gt                5283
_reflns_number_total             7920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201271y_si_001.cif
_cod_data_source_block           4
_cod_original_cell_volume        2646.3(6)
_cod_original_sg_symbol_Hall     '-p 2yb'
_cod_original_sg_symbol_H-M      'p 21/m'
_cod_database_code               4076502