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_4102556
_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 H148 B F24 Mo N11'
_chemical_formula_weight         2475.38
_chemical_name_systematic
; 
 ? 
;
_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                89.7950(10)
_cell_angle_beta                 89.6920(10)
_cell_angle_gamma                70.3280(10)
_cell_formula_units_Z            4
_cell_length_a                   14.9816(3)
_cell_length_b                   20.9091(4)
_cell_length_c                   43.6033(9)
_cell_measurement_reflns_used    9360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.21
_cell_measurement_theta_min      3.02
_cell_volume                     12861.4(5)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (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 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            249480
_diffrn_reflns_theta_full        67.73
_diffrn_reflns_theta_max         67.73
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.575
_exptl_absorpt_correction_T_max  0.7647
_exptl_absorpt_correction_T_min  0.6942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5168
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.292
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3386
_refine_ls_number_reflns         44897
_refine_ls_number_restraints     12556
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0554P)^2^+16.6784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                39928
_reflns_number_total             44897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1008213_si_005.cif
_cod_data_source_block           d09036
_cod_original_cell_volume        12861.4(4)
_cod_database_code               4102556