Tetrahedral iron featuring an appended Lewis acid: distinct pathways for the reduction of hydroxylamine and hydrazine
Kiernicki, John J.; Norwine, Emily E.; Zeller, Matthias; Szymczak, Nathaniel K.; Chemical Communications  (2019) –; doi:10.1039/C9CC05720J

data_7124192
_publ_section_title
;
 Tetrahedral iron featuring an appended Lewis acid: distinct pathways for
 the reduction of hydroxylamine and hydrazine
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05720J
_journal_year                    2019
_chemical_formula_moiety         'C48 H76 B2 Br4 Fe2 N8, 0.409(C H2 Cl2)'
_chemical_formula_sum            'C48.41 H76.82 B2 Br4 Cl0.82 Fe2 N8'
_chemical_formula_weight         1252.83
_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-2018/3
_audit_update_record
;
2019-07-17 deposited with the CCDC.    2019-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                70.8799(10)
_cell_angle_beta                 69.8088(10)
_cell_angle_gamma                65.8643(9)
_cell_formula_units_Z            2
_cell_length_a                   14.0086(4)
_cell_length_b                   14.8635(4)
_cell_length_c                   15.9297(4)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      79.9029
_cell_measurement_theta_min      3.3383
_cell_volume                     2772.76(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'Apex3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev937 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29079
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.739
_diffrn_reflns_theta_min         3.028
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    8.237
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.4085
_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            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       needle
_exptl_crystal_F_000             1278
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.861
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00098(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         11053
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0547P)^2^+4.1772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9165
_reflns_number_total             11053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05720j2.cif
_cod_data_source_block           EN151_0m
_cod_database_code               7124192
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.155
_shelx_estimated_absorpt_t_max   0.734
_shelx_res_checksum              26884