Ruthenium(II)- and osmium(II)-arene-based paullones bearing a TEMPO free-radical unit as potential anticancer drugs
Vladimir B. Arion; Anatolie Dobrov; Simone Goeschl; Michael A. Jakupec; Bernhard K. Keppler; Peter Rapta; Chem.Commun. 48 (2012) 8559–; doi:10.1039/c2cc33786j

data_7108179
_publ_section_title
;
 Ruthenium(II)- and osmium(II)-arene-based paullones bearing a TEMPO
 free-radical unit as potential anticancer drugs
;
_journal_name_full               Chem.Commun.
_journal_page_first              8559
_journal_paper_doi               10.1039/c2cc33786j
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C32 H35 N6 O2, C H4 O'
_chemical_formula_sum            'C33 H39 N6 O3'
_chemical_formula_weight         567.70
_chemical_name_common
;
N-(4-amino-2,2,6,6-tetramethylpiperidinyloxyl)-6-N-(2-
methylaminopyridine)-7,12-dihydroindolo-(3,2-d)(1)benzazepine-9-
carboxamide methanol solvate
;
_chemical_name_systematic
;
N-(4-amino-2,2,6,6-tetramethylpiperidinyloxyl)-6-N-(2-methylaminopyridine)-7,12-
dihydroindolo-[3,2-d][1]benzazepine-9-carboxamide methanol solvate
;
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.778(2)
_cell_length_b                   26.576(3)
_cell_length_c                   12.4884(12)
_cell_measurement_reflns_used    7999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.97
_cell_measurement_theta_min      2.29
_cell_volume                     5900.4(11)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0873
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            66582
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9941
_exptl_absorpt_correction_T_min  0.9793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         3738
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+3.9072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                2927
_reflns_number_total             3738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33786j.txt
_cod_data_source_block           ANDO862
_cod_original_cell_volume        5900.5(11)
_cod_original_sg_symbol_H-M      Iba2
_cod_database_code               7108179