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_4126830
_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_absolute_configuration ad
_chemical_formula_moiety         'C41 H67 B2 Fe N7, C H2 Cl2'
_chemical_formula_sum            'C42 H69 B2 Cl2 Fe N7'
_chemical_formula_weight         820.41
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1611(5)
_cell_length_b                   16.1611(5)
_cell_length_c                   16.5750(6)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.2379
_cell_measurement_theta_min      3.0749
_cell_volume                     4329.1(2)
_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 0.990
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48791
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.363
_diffrn_reflns_theta_min         3.036
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  0.3438
_exptl_absorpt_correction_T_min  0.2849
_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    1.259
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.510
_exptl_crystal_size_min          0.390
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 3135 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         10437
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0452P)^2^+2.9378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                8195
_reflns_number_total             10437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4.cif
_cod_data_source_block           JK2100_0m
_cod_original_cell_volume        4329.1(3)
_cod_database_code               4126830
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.767
_shelx_estimated_absorpt_t_max   0.826
_shelx_res_checksum              54688
_shelx_hkl_checksum              28962