A Novel Homobimetallic Nickel Complex for Asymmetric Direct Mannich Reaction of Imines: A Practical Method on a Multi-Gram Scale
Zhou, Hui; Zhang, Shixiong; Deng, Ping; Zhou, Jing; Liu, Mouxiong; Liang, Guojuan; Xiong, Yan; Chemical Communications  (2017) –; doi:10.1039/C7CC06468C

data_7120864
_publ_section_title
;
 A Novel Homobimetallic Nickel Complex for Asymmetric Direct Mannich
 Reaction of Imines: A Practical Method on a Multi-Gram Scale
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC06468C
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H24 Br N O6 S'
_chemical_formula_sum            'C21 H24 Br N O6 S'
_chemical_formula_weight         498.38
_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-2014/7
_audit_update_record
;
2017-08-07 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7594(11)
_cell_length_b                   12.6345(14)
_cell_length_c                   17.835(2)
_cell_measurement_reflns_used    7387
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.28
_cell_volume                     2199.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24629
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.109
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   0.3375
_exptl_transmission_factor_min   0.2248
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 2012 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+1.4576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.895
_reflns_number_gt                5387
_reflns_number_total             6517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06468c2.cif
_cod_data_source_block           mo_cy_zj2_0m
_cod_database_code               7120864
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.315
_shelx_estimated_absorpt_t_max   0.753
_shelx_res_checksum              24538