Facile Ligand Oxidation and Ring Nitration in Ruthenium Complexes Derived from a Ligand with Dicarboxamide-N and Phosphine-P Donors
Nicole L. Fry; Michael J. Rose; Crystal Nyitray; Pradip K. Mascharak; Inorganic Chemistry 47 (2008) 11604–11610; doi:10.1021/ic801243a

data_4306424
_publ_contact_author_address
;
Department of Chemistry and Biochemistry,
University of California, Santa Cruz,
1156 High Street,
Santa Cruz, CA 95064
USA
;
_publ_contact_author_email       pradip@chemsitry.ucsc.edu
_publ_contact_author_fax         '+1 831 459 2935'
_publ_contact_author_name        'Pradip Mascharak'
_publ_contact_author_phone       '+1 831 459 4251'
_publ_section_title
;
Facile Ligand Oxidation and Ring Nitration in Ruthenium Complexes Derived
from a Ligand with Dicarboxamide-N and Phosphine-P Donors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11604
_journal_page_last               11610
_journal_paper_doi               10.1021/ic801243a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C44 H31 Cl2 N3 O4 P2 Ru, C H Cl3'
_chemical_formula_sum            'C45 H32 Cl5 N3 O4 P2 Ru'
_chemical_formula_weight         1019.00
_chemical_name_common            '[(NO2dppQ)Ru(Cl)2].CHCl3 (2.CHCl3)'
_chemical_name_systematic
; 
 ? 
;
_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                102.117(2)
_cell_angle_beta                 90.025(2)
_cell_angle_gamma                95.669(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5979(16)
_cell_length_b                   13.3799(19)
_cell_length_c                   14.107(2)
_cell_measurement_reflns_used    8385
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.24
_cell_volume                     2129.4(5)
_computing_cell_refinement       'Bruker SAINT v7.34A'
_computing_data_collection       'Bruker APEX-II v2.1-4'
_computing_data_reduction        'Bruker SAINT v7.34A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       \w/2\q-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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23970
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.9238
_exptl_absorpt_correction_T_min  0.8752
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.097
_refine_diff_density_min         -1.612
_refine_diff_density_rms         0.100
_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     622
_refine_ls_number_reflns         10331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0566P)^2^+4.9317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                8243
_reflns_number_total             10331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801243a_si_002_1.cif
_cod_data_source_block           xsc08031
_cod_original_cell_volume        2129.3(5)
_cod_database_code               4306424