Chiral-at-Iron Catalyst: Expanding the Chemical Space for Asymmetric Earth-Abundant Metal Catalysis.
Hong, Yubiao; Jarrige, Lucie; Harms, Klaus; Meggers, Eric; Journal of the American Chemical Society 141 (2019) 4569–4572; doi:10.1021/jacs.9b01352

data_4128954
_publ_section_title
;
 Chiral-at-Iron Catalyst: Expanding the Chemical Space for Asymmetric
 Earth-Abundant Metal Catalysis.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4569
_journal_page_last               4572
_journal_paper_doi               10.1021/jacs.9b01352
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C40 H38 F6 Fe N8, 2(F6 P), 0.75(C4 H8 O), 0.25(C2 H3 N)'
_chemical_formula_sum            'C43.5 H44.75 F18 Fe N8.25 O0.75 P2'
_chemical_formula_weight         1154.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8763(1)
_cell_length_b                   15.3531(2)
_cell_length_c                   24.2529(4)
_cell_measurement_reflns_used    36237
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.36
_cell_measurement_theta_min      3.41
_cell_volume                     4794.58(11)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Piltaus3_SV (STOE, 2016)'
_computing_data_reduction
'X-Area Integrate 1.71.0.0 (STOE, 2016) X-Area LANA 1.68.2.0 (STOE, 2016)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact)'
_computing_publication_material  'X-Area 1.77'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'XT V2014/1 (Bruker AXS Inc., 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            50701
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         75.796
_diffrn_reflns_theta_min         3.407
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.198
_exptl_absorpt_correction_T_max  0.5714
_exptl_absorpt_correction_T_min  0.0895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'STOE LANA, absorption correction by scaling of reflection intensities.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2350
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
; 
 Flack x determined using 3125 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.009(2)
_refine_ls_extinction_coef       0.00020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         9872
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                8379
_reflns_number_total             9872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01352_si_002.cif
_cod_data_source_block           FePyCF3
_cod_original_formula_sum        'C43.50 H44.75 F18 Fe N8.25 O0.75 P2'
_cod_database_code               4128954
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.321
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              86891
_shelx_hkl_checksum              19437