Chiral Tripodal Ligand Containing Three N-Heterocyclic Donor Functions and Its Copper Complexes: Crystallization of [LCuI]22+/[L2CuII]2+ Stereoisomers and Tyrosinase Activity
Aline Arnold; Christian Limberg; Ramona Metzinger; Inorganic Chemistry 51 (2012) 12210–12217; doi:10.1021/ic301391s

data_4331012
_publ_contact_author_address
;
      Institut fuer Chemie
      Humboldt Universitaet zu Berlin
      Brook-Taylor-Str. 2
      12489 Berlin
      Germany
;
_publ_contact_author_email       ramona.metzinger@chemie.hu-berlin.de
_publ_contact_author_fax         0049-30-20936966
_publ_contact_author_name        'Ramona Metzinger'
_publ_contact_author_phone       0049-30-20937391
_publ_section_title
;
 Chiral Tripodal Ligand Containing Three N-Heterocyclic Donor Functions
 and Its Copper Complexes: Crystallization of [LCuI]22+/[L2CuII]2+
 Stereoisomers and Tyrosinase Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12210
_journal_page_last               12217
_journal_paper_doi               10.1021/ic301391s
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C55 H50 Cu2 F3 N10 O7 S, C F3 O3 S, C4 H10 O, C2 H3 N'
_chemical_formula_sum            'C62 H63 Cu2 F6 N11 O11 S2'
_chemical_formula_weight         1443.43
_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                 91.046(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0535(5)
_cell_length_b                   17.6171(13)
_cell_length_c                   33.4948(19)
_cell_measurement_reflns_used    13424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      3.21
_cell_volume                     6521.4(7)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'PLATON, 1990'
_computing_publication_material  'PLATON, 1990'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,319 exposures'
_diffrn_radiation_collimation    '0.5 mm diameter monocapillary'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'long fine focus sealed x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            89221
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       needle
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         12809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0621P)^2^+9.3406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1508
_reflns_number_gt                10033
_reflns_number_total             12809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301391s_si_001_6.cif
_cod_data_source_block           moni133_2_complex5
_cod_database_code               4331012