Bonding and Activation of N2 in Mo(0) Complexes Supported by Hybrid Tripod Ligands with Mixed Dialkylphosphine/Diarylphosphine Donor Groups: Interplay of Steric and Electronic Factors
Ludger Söncksen; Christian Gradert; Jan Krahmer; Christian Näther; Felix Tuczek; Inorganic Chemistry 52 (2013) 6576–6589; doi:10.1021/ic400582v

data_4335105
_publ_section_title
;
 Bonding and Activation of N2 in Mo(0) Complexes Supported by Hybrid
 Tripod Ligands with Mixed Dialkylphosphine/Diarylphosphine Donor Groups:
 Interplay of Steric and Electronic Factors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6576
_journal_page_last               6589
_journal_paper_doi               10.1021/ic400582v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C60 H65 Mo P5'
_chemical_formula_weight         1036.91
_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                 95.107(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3476(7)
_cell_length_b                   25.3230(19)
_cell_length_c                   18.3494(12)
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.31
_cell_volume                     5714.7(7)
_computing_cell_refinement       'STOE IPDS-1 program package'
_computing_data_collection       'STOE IPDS-1 program package'
_computing_data_reduction        'STOE IPDS-1 program package'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi scan'
_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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59603
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_void_count_electrons
;
         1     0.279     0.234     0.103     229.2       9.3
         2     0.279     0.266     0.604     225.3      11.0
         3     0.721     0.734     0.396     228.9      10.1
         4     0.721     0.766     0.896     225.6      10.1
;
_platon_squeeze_void_volume      910.7
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0065(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         12112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0819
_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^)+(0.0099P)^2^+42.7041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1838
_reflns_number_gt                10505
_reflns_number_total             12112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400582v_si_003.cif
_cod_data_source_block           felix98
_cod_database_code               4335105