Synthesis, Protonation, and Reduction of Ruthenium-Peroxo Complexes with Pendent Nitrogen Bases
Tristan A. Tronic; Werner Kaminsky; Michael K. Coggins; James M. Mayer; Inorganic Chemistry 51 (2012) 10916–10928; doi:10.1021/ic3013987

data_4330658
_publ_contact_author_address
;
Department of Chemistry
University of Washington
Seattle
Washington, 98195, USA
;
_publ_contact_author_email       kaminsky@chem.washington.edu
_publ_contact_author_fax         00(206)6858665
_publ_contact_author_name        'Werner Kaminsky'
_publ_contact_author_phone       00(206)5437585
_publ_section_title
;
 Synthesis, Protonation, and Reduction of Ruthenium-Peroxo Complexes with
 Pendent Nitrogen Bases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10916
_journal_page_last               10928
_journal_paper_doi               10.1021/ic3013987
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C40 H47 N2 O2 P2 Ru, 0.33(C6 H14), C F3 O3 S, 0.67(C H2 Cl2)'
_chemical_formula_sum            'C43.65 H52.96 Cl1.34 F3 N2 O5 P2 Ru S'
_chemical_formula_weight         985.21
_chemical_name_common            tt4115
_chemical_name_systematic
;
 tt4115
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-04-11T11:14:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.688(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.413(3)
_cell_length_b                   13.9781(10)
_cell_length_c                   25.488(2)
_cell_measurement_reflns_used    360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     8992.4(14)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            141832
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.9043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       prism
_exptl_crystal_F_000             4069
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.408
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         11462
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+31.9762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                8331
_reflns_number_total             11462
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3013987_si_002_07.cif
_cod_data_source_block           CpRuPPhNBnO2
_cod_original_cell_volume        8992.5(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4330658