Using the Ni-[(benzylprolyl)amino]benzophenone complex in the Glaser reaction for the synthesis of bis α-amino acids
Mkrtchyan, Anna F.; Hayriyan, Liana A.; Karapetyan, Ani J.; Tovmasyan, Anna S.; Tsaturyan, Avetis H.; Khrustalev, Victor N.; Maleev, Viktor I.; Saghyan, Ashot S.; New Journal of Chemistry 44 (2020) 11927–11932; doi:10.1039/D0NJ02072A

data_7059696
_publ_section_title
;
 Using the Ni-[(benzylprolyl)amino]benzophenone complex in the Glaser
 reaction for the synthesis of bis \a-amino acids
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11927
_journal_page_last               11932
_journal_paper_doi               10.1039/D0NJ02072A
_journal_volume                  44
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C60 H52 N6 Ni2 O6'
_chemical_formula_sum            'C60 H52 N6 Ni2 O6'
_chemical_formula_weight         1070.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-10-14 deposited with the CCDC.	2020-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.884(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.983(3)
_cell_length_b                   12.994(3)
_cell_length_c                   33.620(7)
_cell_measurement_reflns_used    8352
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.14
_cell_measurement_theta_min      2.22
_cell_volume                     5669(2)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_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  0.0704
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            56162
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.507
_diffrn_reflns_theta_min         0.606
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       prism
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.08(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1286
_refine_ls_number_reflns         23063
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.096P)^2^+3.93P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.1998
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                17022
_reflns_number_total             23063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02072a2.cif
_cod_data_source_block           3a_sq
_cod_depositor_comments
;Adding full bibliography for 7059696.cif.

 Adding full bibliography for 7059696.cif.
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7059696
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.870
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              37605
_shelx_fab_checksum              51531