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_4330347
_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 H78 Cl2 N4 P4 Ru2, 4(C H Cl3), 2(B F4)'
_chemical_formula_sum            'C36 H82 B2 Cl14 F8 N4 P4 Ru2'
_chemical_formula_weight         1567.00
_chemical_name_common            '[(HPNPRuCl)2(H2NNH2)](BF4)2 (3a)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                83.049(2)
_cell_angle_beta                 80.921(2)
_cell_angle_gamma                67.533(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8002(4)
_cell_length_b                   13.2180(4)
_cell_length_c                   22.3853(7)
_cell_measurement_reflns_used    9624
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.34
_cell_volume                     3179.05(18)
_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-97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27428
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  0.9760
_exptl_absorpt_correction_T_min  0.8104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       needle
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         11647
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0666P)^2^+14.1693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                7701
_reflns_number_total             11647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3010322_si_001_02.cif
_cod_data_source_block           srd589
_cod_original_cell_volume        3179.06(18)
_cod_database_code               4330347