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_1550983
_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_formula_moiety         'C18 H36 K N2 O6, C41 H65 B2 Fe N5'
_chemical_formula_sum            'C59 H101 B2 Fe K N7 O6'
_chemical_formula_weight         1121.03
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_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
_audit_update_record
;
2018-12-10 deposited with the CCDC.    2019-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                67.321(5)
_cell_angle_beta                 71.202(5)
_cell_angle_gamma                89.815(4)
_cell_formula_units_Z            4
_cell_length_a                   19.503(3)
_cell_length_b                   21.623(3)
_cell_length_c                   22.147(4)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.9829
_cell_measurement_theta_min      2.9857
_cell_volume                     8079(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-2017/1 (Sheldrick, 2015, 2017), 
SHELXLE Rev859 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.939
_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  0.0528
_diffrn_reflns_av_unetI/netI     0.1100
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            70366
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.864
_diffrn_reflns_theta_min         2.488
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_correction_T_min  0.4459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.
(2015). J. Appl. Cryst. 48 3-10.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.922
_exptl_crystal_description       plate
_exptl_crystal_F_000             2428
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.043(2)
_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   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2089
_refine_ls_number_reflns         70366
_refine_ls_number_restraints     3477
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1805
_refine_ls_R_factor_gt           0.1316
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2025P)^2^+20.2700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3677
_refine_ls_wR_factor_ref         0.4104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                41234
_reflns_number_total             70366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00561g2.cif
_cod_data_source_block           jk2200_0m_5_sq
_cod_database_code               1550983
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              51112
_shelx_fab_checksum              36622