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_1550980
_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_sum            'C39 H51 Fe N5 S2'
_chemical_formula_weight         709.81
_chemical_name_systematic        (butylPDPtBu)Fe(SPh)2
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
;
2019-03-15 deposited with the CCDC.    2019-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.373(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2208(10)
_cell_length_b                   15.9972(18)
_cell_length_c                   25.443(3)
_cell_measurement_reflns_used    4560
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      78.5577
_cell_measurement_theta_min      3.2638
_cell_volume                     3746.5(7)
_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 Rev946 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest CMOS diffractometer with PhotonII charge-integrating pixel 
array detector (CPAD)
;
_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  0.0582
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20041
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.877
_diffrn_reflns_theta_min         3.265
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    4.521
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.4964
_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    1.258
_exptl_crystal_description       needle
_exptl_crystal_F_000             1512
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / n-pentane'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         7782
_refine_ls_number_restraints     1218
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1001P)^2^+0.4014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5293
_reflns_number_total             7782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00561g2.cif
_cod_data_source_block           JK566_0m
_cod_database_code               1550980
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.450
_shelx_estimated_absorpt_t_max   0.915
_shelx_res_checksum              83223