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_4126836
_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         'C41 H63 B2 Cl2 Fe N5'
_chemical_formula_sum            'C41 H63 B2 Cl2 Fe N5'
_chemical_formula_weight         774.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.716(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8752(6)
_cell_length_b                   20.4520(6)
_cell_length_c                   10.2304(5)
_cell_measurement_reflns_used    8844
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.5200
_cell_measurement_theta_min      2.2890
_cell_volume                     4130.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'abstract diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1381
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            63184
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.730
_diffrn_reflns_theta_min         2.238
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 10
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    4.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.00041(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+4.3280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5482
_reflns_number_total             7716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1-Cl.cif
_cod_data_source_block           jk1191a
_cod_database_code               4126836
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.811
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              960
_shelx_hkl_checksum              41685