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_4330346
_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         'C32 H74 Cl2 N6 P4 Ru2, 2(B F4), C H2 Cl2'
_chemical_formula_sum            'C33 H76 B2 Cl4 F8 N6 P4 Ru2'
_chemical_formula_weight         1198.44
_chemical_name_common            '[HPNPRu(N2)Cl]2(BF4)2 (2)'
_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                 104.3220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7122(5)
_cell_length_b                   14.9191(5)
_cell_length_c                   22.5318(8)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.55
_cell_volume                     5117.6(3)
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26860
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       needle
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         9376
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+2.9614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                8090
_reflns_number_total             9460
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3010322_si_001_01.cif
_cod_data_source_block           srd390
_cod_database_code               4330346