Bimetallic Ruthenium PNP Pincer Complex As a Platform to Model Proposed Intermediates in Dinitrogen Reduction to Ammonia
Sergio S. Rozenel; John Arnold; Inorganic Chemistry 51 (2012) 9730–9739; doi:10.1021/ic3010322

data_4330354
_publ_section_title
;
 Bimetallic Ruthenium PNP Pincer Complex As a Platform to Model Proposed
 Intermediates in Dinitrogen Reduction to Ammonia
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9730
_journal_page_last               9739
_journal_paper_doi               10.1021/ic3010322
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C33 H74 Cl2 F3 N2 O3 P4 Ru2 S, C F3 O3 S'
_chemical_formula_sum            'C34 H74 Cl2 F6 N2 O6 P4 Ru2 S2'
_chemical_formula_weight         1181.99
_chemical_name_common            '[(HPNPRu)2(Cl)2(SO3CF3)]SO3CF3 (9)'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.049(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.242(2)
_cell_length_b                   34.018(8)
_cell_length_c                   14.882(3)
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    144(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.28
_cell_volume                     5051.2(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SIR-2004
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      144(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'phi and omega 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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60667
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.8919
_exptl_absorpt_correction_T_min  0.8440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+5.7858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                7842
_reflns_number_total             9286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3010322_si_001_09.cif
_cod_data_source_block           srd412
_cod_original_cell_volume        5051(2)
_cod_database_code               4330354