Reduction of Dinitrogen to Ammonia Catalyzed by Molybdenum Diamido Complexes.
Wickramasinghe, Lasantha A.; Schrock, Richard R.; Müller, Peter; Ogawa, Takaya; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b04800

data_4126242
_publ_section_title
;
 Reduction of Dinitrogen to Ammonia Catalyzed by Molybdenum Diamido
 Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b04800
_journal_year                    2017
_chemical_formula_sum            'C39 H46 F5 Mo N4 O1.5'
_chemical_formula_weight         785.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014/6
_cell_angle_alpha                96.1815(15)
_cell_angle_beta                 99.3959(15)
_cell_angle_gamma                90.7841(15)
_cell_formula_units_Z            8
_cell_length_a                   17.0362(15)
_cell_length_b                   19.2201(17)
_cell_length_c                   23.935(2)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.47
_cell_measurement_theta_min      2.28
_cell_volume                     7683.2(12)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1073
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            194136
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.212
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.745
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1876
_refine_ls_number_reflns         29182
_refine_ls_number_restraints     3005
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+5.9938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19158
_reflns_number_total             29182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04800_si_001.cif
_cod_data_source_block           X16199
_cod_original_cell_volume        7683.4(12)
_cod_original_formula_sum        'C39 H46 F5 Mo N4 O1.50'
_cod_database_code               4126242
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2014/6
_shelx_res_checksum              357
_shelx_hkl_checksum              14044