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_4306425
_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 H32 Cl2 N2 O2 P2 Ru'
_chemical_formula_sum            'C44 H32 Cl2 N2 O2 P2 Ru'
_chemical_formula_weight         854.63
_chemical_name_common            '[(dppQ)Ru(Cl)2] (1)'
_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                 105.959(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8868(15)
_cell_length_b                   15.8457(18)
_cell_length_c                   18.982(2)
_cell_measurement_reflns_used    1861
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.03
_cell_measurement_theta_min      2.80
_cell_volume                     3726.7(7)
_computing_cell_refinement       'Bruker SAINT v7.33A'
_computing_data_collection       'Bruker APEX-II v2.1'
_computing_data_reduction        'Bruker SAINT v7.33A'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       \w/2\q-scans
_diffrn_radiation_monochromator  'channel-cut Si-<111> crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.1368
_diffrn_reflns_av_sigmaI/netI    0.1121
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36318
_diffrn_reflns_theta_full        29.03
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.9914
_exptl_absorpt_correction_T_min  0.9263
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, 2004'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0040(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                4117
_reflns_number_total             7648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801243a_si_002_2.cif
_cod_data_source_block           xsc07101
_cod_original_cell_volume        3726.8(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4306425