Synthesis of [(DPPNCH2CH2)3N]3- Molybdenum Complexes (DPP = 3,5-(2,5-Diisopropylpyrrolyl)2C6H3) and Studies Relevant to Catalytic Reduction of Dinitrogen
Michael R. Reithofer; Richard R. Schrock; Peter Müller; Journal of the American Chemical Society 132 (2010) 8349–8358; doi:10.1021/ja1008213

data_4102557
_publ_section_title
;
 Synthesis of [(DPPNCH2CH2)3N]3- Molybdenum Complexes (DPP =
 3,5-(2,5-Diisopropylpyrrolyl)2C6H3) and Studies Relevant to Catalytic
 Reduction of Dinitrogen
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8349
_journal_page_last               8358
_journal_paper_doi               10.1021/ja1008213
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C134.5 H167 B F24 Mo N12'
_chemical_formula_weight         2514.55
_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                 102.4510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5735(3)
_cell_length_b                   30.3139(6)
_cell_length_c                   31.0683(6)
_cell_measurement_reflns_used    9664
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.42
_cell_measurement_theta_min      2.91
_cell_volume                     13402.5(5)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            243120
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.7511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5284
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1650
_refine_ls_number_reflns         24557
_refine_ls_number_restraints     3155
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0764P)^2^+21.8813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                18888
_reflns_number_total             24557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1008213_si_006.cif
_cod_data_source_block           d10016
_cod_original_formula_sum        'C134.50 H167 B F24 Mo N12'
_cod_database_code               4102557