Macrocyclic Salen‒Bis-NHC Hybrid Ligands and Their Application to the Synthesis of Enantiopure Bi- and Trimetallic Complexes
Mechler, Melanie; Frey, Wolfgang; Peters, René; Organometallics 33 (2014) 5492–; doi:10.1021/om500762r

data_4084359
_publ_section_title
;
 Macrocyclic Salen--Bis-NHC Hybrid Ligands and Their Application to the
 Synthesis of Enantiopure Bi- and Trimetallic Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5492
_journal_paper_doi               10.1021/om500762r
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C48.5 H53 Au2 Cl3 N6 Ni O2'
_chemical_formula_weight         1310.96
_chemical_name_systematic        15-Ni
_space_group_IT_number           1
_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                77.468(8)
_cell_angle_beta                 72.261(7)
_cell_angle_gamma                66.012(6)
_cell_formula_units_Z            2
_cell_length_a                   12.2291(17)
_cell_length_b                   13.6366(19)
_cell_length_c                   16.584(2)
_cell_measurement_reflns_used    9219
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.64
_cell_volume                     2392.8(6)
_computing_cell_refinement       'Bruker APEXII Software Suite, 2008'
_computing_data_collection       'Bruker APEXII Software Suite, 2008'
_computing_data_reduction        'Bruker APEXII Software Suite, 2008'
_computing_molecular_graphics    'SHELXTL-plus, XP (SHeldrick, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_sigmaI/netI    0.1313
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39507
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.718
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.2524
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1278
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.747
_refine_diff_density_min         -4.759
_refine_diff_density_rms         0.384
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_coef       0.0029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1056
_refine_ls_number_reflns         15365
_refine_ls_number_restraints     1030
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1780
_refine_ls_R_factor_gt           0.1092
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0925P)^2^+178.5674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2575
_refine_ls_wR_factor_ref         0.2859
_reflns_number_gt                9219
_reflns_number_total             15365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500762r_si_002.cif
_cod_data_source_block           s2042lm
_cod_depositor_comments
'Adding full bibliography for 4084357--4084359.cif.'
_cod_original_formula_sum        'C48.50 H53 Au2 Cl3 N6 Ni O2'
_cod_database_code               4084359