NHC and nucleophile chelation effects on reactive iron(ii) species in alkyl-alkyl cross-coupling.
Fleischauer, Valerie E.; Muñoz Iii, Salvador B; Neate, Peter G. N.; Brennessel, William W.; Neidig, Michael L.; Chemical science 9 (2018) 1878–1891; doi:10.1039/c7sc04750a

data_1548640
_publ_section_title
;
 NHC and nucleophile chelation effects on reactive iron(ii) species in
 alkyl-alkyl cross-coupling.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              1878
_journal_page_last               1891
_journal_paper_doi               10.1039/c7sc04750a
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H46 Fe N2 O4'
_chemical_formula_sum            'C33 H46 Fe N2 O4'
_chemical_formula_weight         590.57
_chemical_name_common            neism35
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-05-24 deposited with the CCDC.
2018-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8779(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2603(6)
_cell_length_b                   22.9235(12)
_cell_length_c                   16.1864(9)
_cell_measurement_reflns_used    3961
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      35.17
_cell_measurement_theta_min      2.59
_cell_volume                     4056.2(4)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            89669
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.797
_diffrn_reflns_theta_min         1.777
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.7065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2016a)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.967
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
; 
 Flack x determined using 7862 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.017(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         22458
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.963
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                18509
_reflns_number_total             22458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04750a2.cif
_cod_data_source_block           neism35
_cod_depositor_comments
'Adding full bibliography for 1548638--1548640.cif.'
_cod_database_code               1548640
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.882
_shelx_res_checksum              66744
_shelx_fab_checksum              84867