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_4083144
_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, 2.49(H2 O)'
_chemical_formula_sum            'C54 H52.97 N6 Ni2 O8.49'
_chemical_formula_weight         1039.15
_chemical_name_systematic
; 
(2S,2'R)-bis-N-[alpha-{2-[1-benzyl(pyrrolidine-2-yl)
carbonylamino]phenyl}benzylidene]glycinato-(N,N,N,O) 
nickel
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1460(3)
_cell_length_b                   13.9307(2)
_cell_length_c                   26.5845(5)
_cell_measurement_reflns_used    20726
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      71.64
_cell_measurement_theta_min      3.58
_cell_volume                     4868.50(16)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      '1126 frames, detector distance 42 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  0.0784
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20870
_diffrn_reflns_theta_full        71.90
_diffrn_reflns_theta_max         71.90
_diffrn_reflns_theta_min         3.58
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2171.4
_exptl_crystal_preparation
'crystallization from aceton/chloroform mixture'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack (1983), 4256 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_coef       0.00025(6)
_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   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         8895
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0655P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                5523
_reflns_number_total             8895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500034x_si_001.cif
_cod_data_source_block           ni_dimer
_cod_database_code               4083144