Hydrazine Capture and N-N Bond Cleavage at Iron Enabled by Flexible Appended Lewis Acids.
Kiernicki, John J.; Zeller, Matthias; Szymczak, Nathaniel K.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b11465

data_4126829
_publ_section_title
;
 Hydrazine Capture and N-N Bond Cleavage at Iron Enabled by Flexible
 Appended Lewis Acids.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11465
_journal_year                    2017
_chemical_formula_moiety
'C53 H79 B2 Fe N7 O2, 0.783(C6 H6 O), 0.217(C6 H6)'
_chemical_formula_sum            'C59 H85 B2 Fe N7 O2.78'
_chemical_formula_weight         1014.33
_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-2017/1
_cell_angle_alpha                105.865(3)
_cell_angle_beta                 105.194(2)
_cell_angle_gamma                105.175(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8379(9)
_cell_length_b                   16.9517(11)
_cell_length_c                   19.8869(15)
_cell_measurement_reflns_used    9138
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.5955
_cell_measurement_theta_min      2.8561
_cell_volume                     3165.3(4)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2016)'
_computing_data_collection       'Apex3 v2016.9-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker, 2016)'
_computing_structure_refinement
;  
SHELXL-2016/6 (Sheldrick, 2015, 2016), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            83767
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       plate
_exptl_crystal_F_000             1093
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0103(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         15586
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+6.5658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12607
_reflns_number_total             15586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            5-OPh.cif
_cod_data_source_block           jk298_0m_sq
_cod_database_code               4126829
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              2223
_shelx_hkl_checksum              10106
_shelx_fab_checksum              2217