Tuning ligand field strength with pendent Lewis acids: access to high spin iron hydrides
Kiernicki, John J.; Shanahan, James P.; Zeller, Matthias; Szymczak, Nathaniel K.; Chemical Science  (2019) –; doi:10.1039/C9SC00561G

data_1550972
_publ_section_title
;
 Tuning ligand field strength with pendent Lewis acids: access to high
 spin iron hydrides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00561G
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C41 H65 B2 Fe N5, 0.892(C7 H8)'
_chemical_formula_sum            'C47.24 H72.13 B2 Fe N5'
_chemical_formula_weight         787.61
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_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     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-12-10 deposited with the CCDC.    2019-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0995(5)
_cell_length_b                   16.0995(5)
_cell_length_c                   16.3816(5)
_cell_measurement_reflns_used    8849
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.1580
_cell_measurement_theta_min      3.8830
_cell_volume                     4246.0(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-2018/1 (Sheldrick, 2015, 2018), 
SHELXLE Rev882 (H\"ubschle et al., 2011)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_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  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30458
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.949
_diffrn_reflns_theta_min         3.850
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    3.132
_exptl_absorpt_correction_T_max  0.5259
_exptl_absorpt_correction_T_min  0.4269
_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            black
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       cube
_exptl_crystal_F_000             1706
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.390(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         4559
_refine_ls_number_restraints     668
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0561
_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^)+(0.1148P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1651
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                3416
_reflns_number_total             4559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00561g2.cif
_cod_data_source_block           JK3155_0m
_cod_original_cell_volume        4246.0(3)
_cod_database_code               1550972
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.745
_shelx_res_checksum              76701