Oxidative dehydrogenation of an amine group of a macrocyclic ligand in the coordination sphere of a CuII complex
Christian, Gemma J.; Arbuse, Arnau; Fontrodona, Xavier; Martinez, Ma Angeles; Llobet, Antoni; Maseras, Feliu; Dalton Transactions  (2009) 6013–6020; doi:10.1039/b902947h

data_7001744
_publ_section_title
;
 Oxidative dehydrogenation of an amine group of a macrocyclic ligand in
 the coordination sphere of a CuII complex
;
_journal_issue                   30
_journal_name_full               'Dalton Transactions'
_journal_page_first              6013
_journal_page_last               6020
_journal_paper_doi               10.1039/b902947h
_journal_year                    2009
_chemical_formula_moiety
'(C40 H52 Cu2 N8), 0.5(C4 H10 O), 2(C F3 O3 S), (C2 H3 N), (O H2)'
_chemical_formula_sum            'C46 H62 Cu2 F6 N9 O7.5 S2'
_chemical_formula_weight         1166.25
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.086(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.413(6)
_cell_length_b                   19.459(9)
_cell_length_c                   21.578(10)
_cell_measurement_reflns_used    7109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.36
_cell_volume                     5172(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            78199
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+2.0361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                11011
_reflns_number_total             12727
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902947h.txt
_cod_data_source_block           aafp241g
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C46 H62 Cu2 F6 N9 O7.50 S2'
_cod_database_code               7001744