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_1550974
_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         'C53 H74 B2 Fe N5 P2, 3(C4 H8 O)'
_chemical_formula_sum            'C65 H98 B2 Fe N5 O3 P2'
_chemical_formula_weight         1136.89
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-10 deposited with the CCDC.    2019-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                92.678(16)
_cell_angle_beta                 91.124(18)
_cell_angle_gamma                114.185(16)
_cell_formula_units_Z            2
_cell_length_a                   10.989(6)
_cell_length_b                   12.928(6)
_cell_length_c                   24.431(11)
_cell_measurement_reflns_used    6387
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.3335
_cell_measurement_theta_min      2.3185
_cell_volume                     3160(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'Apex3 v2017.3-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev915 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.978
_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  0.1415
_diffrn_reflns_av_unetI/netI     0.1800
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33481
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5095
_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            block
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       yellow
_exptl_crystal_F_000             1226
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         11734
_refine_ls_number_restraints     401
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.2633
_refine_ls_R_factor_gt           0.1288
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2373P)^2^+3.0900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3444
_refine_ls_wR_factor_ref         0.4225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4754
_reflns_number_total             11734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00561g2.cif
_cod_data_source_block           jk319
_cod_database_code               1550974
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              87