Facile Isolation of Bisimines Based on 3,3'-Diaminobenzidine: Direct Access to Unsymmetrical Bimetallic Salphen Building Blocks
Simona Curreli; Eduardo C. Escudero-Adán; Jordi Benet-Buchholz; Arjan W. Kleij; Journal of Organic Chemistry 72 (2007) 7018–7021; doi:10.1021/jo070696f

data_4024127
_publ_section_title
;
 Facile Isolation of Bisimines Based on 3,3'-Diaminobenzidine:
 Direct Access to Unsymmetrical Bimetallic Salphen Building Blocks
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7018
_journal_page_last               7021
_journal_paper_doi               10.1021/jo070696f
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C74 H94 N8 O7 S3'
_chemical_formula_weight         1303.75
_space_group_IT_number           2
_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                95.385(5)
_cell_angle_beta                 91.957(5)
_cell_angle_gamma                100.719(5)
_cell_formula_units_Z            2
_cell_length_a                   10.6521(9)
_cell_length_b                   12.8865(11)
_cell_length_c                   25.943(2)
_cell_measurement_reflns_used    6596
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.04
_cell_measurement_theta_min      3.04
_cell_volume                     3478.7(5)
_computing_cell_refinement       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_collection       'Bruker-Nonius Apex v1.0-22 2002'
_computing_data_reduction        'SAINT+ Version 7.06A Bruker-Nonius, 2004'
_computing_molecular_graphics    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_publication_material  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_refinement  'Shelxtl Version 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'Shelxtl Version 6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.815
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1078
_diffrn_reflns_av_sigmaI/netI    0.1393
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            43309
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.73
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           90
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.868031
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2.1 2003 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         16515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2244
_refine_ls_wR_factor_ref         0.2661
_reflns_number_gt                9732
_reflns_number_total             16515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo070696f-File001.cif
_cod_data_source_block           awk117_0m
_cod_database_code               4024127