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_4335104
_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            'C40 H57 Mo N2 P5'
_chemical_formula_weight         816.67
_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                 106.032(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3102(9)
_cell_length_b                   18.5529(9)
_cell_length_c                   20.8163(18)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      10
_cell_volume                     4569.3(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36756
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.9564
_exptl_absorpt_correction_T_min  0.8215
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
X-Red and X-Shape, STOE & CIE, Darmstadt, Germany) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_platon_squeeze_void_count_electrons
;
         1     0.000     0.500     1.000     343.2      80.0
         2     0.500     0.000     0.500     343.2      80.5
;
_platon_squeeze_void_volume      694.5
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.0045(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   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8862
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0563P)^2^+0.0182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                7566
_reflns_number_total             8862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400582v_si_002.cif
_cod_data_source_block           felix91
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4335104