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_4330661
_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         'C34 H51 Cl N2 P2 Ru, C7 H8'
_chemical_formula_sum            'C41 H59 Cl N2 P2 Ru'
_chemical_formula_weight         778.36
_chemical_name_common            tt_3_219
_chemical_name_systematic
;
 tt_3_219
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_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             2012-04-11T10:31:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                93.416(2)
_cell_angle_beta                 102.043(2)
_cell_angle_gamma                106.753(2)
_cell_formula_units_Z            4
_cell_length_a                   11.8320(5)
_cell_length_b                   17.2336(6)
_cell_length_c                   20.2054(8)
_cell_measurement_reflns_used    350
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3826.7(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.984
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            158277
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         30.73
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.9321
_exptl_absorpt_correction_T_min  0.9057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         23413
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+3.2010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                19582
_reflns_number_total             23413
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3013987_si_002_10.cif
_cod_data_source_block           CpRuPtBuNPhCl
_cod_database_code               4330661