Chiral Nickel(II) Binuclear Complexes: Targeted Diastereoselective Electrosynthesis
Magdesieva, Tatiana V.; Levitskiy, Oleg A.; Grishin, Yuri K.; Ambartsumyan, Asmik A.; Paseshnichenko, Ksenia A.; Kolotyrkina, Natalia G.; Kochetkov, Konstantin A.; Organometallics 33 (2014) 4639–; doi:10.1021/om500034x

data_4083145
_publ_contact_author             'Dr Ksenia A. Paseshnichenko'
_publ_section_title
;
 Chiral Nickel(II) Binuclear Complexes: Targeted Diastereoselective
 Electrosynthesis
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4639
_journal_paper_doi               10.1021/om500034x
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C54 H48 N6 Ni2 O6, 0.32(C3 H8 O), 0.27(C2 H6 O)'
_chemical_formula_sum            'C55.52 H52.24 N6 Ni2 O6.6'
_chemical_formula_weight         1026.49
_chemical_name_systematic
;
(2S,2'S)-bis-N-[alpha-{2-[1-benzyl(pyrrolidine-2-yl)
carbonylamino]phenyl}benzylidene]glycinato-(N,N,N,O) 
nickel
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.0814(2)
_cell_length_b                   18.7855(2)
_cell_length_c                   37.6820(6)
_cell_measurement_reflns_used    3345
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      39.73
_cell_measurement_theta_min      8.13
_cell_volume                     9967.9(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      '2274 frames, detector distance 80 mm'
_diffrn_measurement_device_type  'Stoe STADI VARI'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  none
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            56195
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         66.407
_diffrn_reflns_theta_min         3.322
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4289.3
_exptl_crystal_preparation
'crystallization from i-propanol/ethanol/acetonitrile mixture'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 4371 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.035(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1305
_refine_ls_number_reflns         17306
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+2.5407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.810
_reflns_number_gt                12373
_reflns_number_total             17306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500034x_si_001.cif
_cod_data_source_block           ni_2
_cod_original_formula_sum        'C55.52 H52.24 N6 Ni2 O6.60'
_cod_database_code               4083145