Synthesis of Biologically Relevant Compounds by Ruthenium Porphyrin Catalyzed Amination of Benzylic C‒H Bonds
Zardi, Paolo; Caselli, Alessandro; Macchi, Piero; Ferretti, Francesco; Gallo, Emma; Organometallics 33 (2014) 2210–; doi:10.1021/om500064d

data_4083090
_publ_section_title
;
 Synthesis of Biologically Relevant Compounds by Ruthenium Porphyrin
 Catalyzed Amination of Benzylic C--H Bonds
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2210
_journal_paper_doi               10.1021/om500064d
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C177 H126 Cl2 F48 N12 O8 Ru2'
_chemical_formula_weight         3733.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-12-19T10:11:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 111.456(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   47.9884(9)
_cell_length_b                   15.0488(4)
_cell_length_c                   25.7745(5)
_cell_measurement_reflns_used    10997
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.705
_cell_measurement_theta_min      1.82
_cell_volume                     17323.6(7)
_computing_cell_refinement
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0017434
_diffrn_orient_matrix_UB_12      -0.046653
_diffrn_orient_matrix_UB_13      0.0037288
_diffrn_orient_matrix_UB_21      0.0152122
_diffrn_orient_matrix_UB_22      0.0061337
_diffrn_orient_matrix_UB_23      0.0174109
_diffrn_orient_matrix_UB_31      -0.0042171
_diffrn_orient_matrix_UB_32      0.0028641
_diffrn_orient_matrix_UB_33      0.0236012
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.1088
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            63431
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.574
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.83034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_F_000             7560
_exptl_crystal_size_max          0.3102
_exptl_crystal_size_mid          0.1389
_exptl_crystal_size_min          0.0194
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         15717
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+69.7800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                10050
_reflns_number_total             15717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500064d_si_001.cif
_cod_data_source_block           compound7
_cod_depositor_comments
'Adding full bibliography for 4083089--4083090.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4083090