Shining Light on Dinitrogen Cleavage: Structural Features, Redox Chemistry, and Photochemistry of the Key Intermediate Bridging Dinitrogen Complex
John J. Curley; Timothy R. Cook; Steven Y. Reece; Peter Müller; Christopher C. Cummins; Journal of the American Chemical Society 130 (2008) 9394–9405; doi:10.1021/ja8002638

data_4108074
_publ_contact_author_address
;Massachusetts Institute of Technology
77 Massachusetts Avenue
Cambridge, MA
02139
6-435
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_name        'Christopher C. Cummins'
_publ_section_title
;
 Shining Light on Dinitrogen Cleavage: Structural Features, Redox
 Chemistry, and Photochemistry of the Key Intermediate Bridging Dinitrogen
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9394
_journal_page_last               9405
_journal_paper_doi               10.1021/ja8002638
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C158.4 H178.4 B2 F48 Mo2 N8 O4.4'
_chemical_formula_weight         3390.19
_chemical_name_common            'compound 2[B(ArF)4]2 in main text'
_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                 96.2580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.0959(10)
_cell_length_b                   21.8610(12)
_cell_length_c                   21.5744(12)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.33
_cell_volume                     8015.0(8)
_computing_cell_refinement       'SAINT 7 (Bruker-AXS, 2005)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 7 (Bruker-AXS, 2005)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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       'omega and phi scans'
_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  0.0812
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            141474
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.9737
_exptl_absorpt_correction_T_min  0.9610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             3492
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.253
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         16389
_refine_ls_number_restraints     1206
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0618P)^2^+12.7639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                11975
_reflns_number_total             16389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8002638-file001_5.cif
_cod_data_source_block           06247_0m
_cod_original_formula_sum        'C158.40 H178.40 B2 F48 Mo2 N8 O4.40'
_cod_database_code               4108074