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_1548638
_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_formula_moiety         'C26.71 H34.57 Br1.14 Fe N2 O1.86, C4 H10 O'
_chemical_formula_sum            'C30.71 H44.57 Br1.14 Fe N2 O2.86'
_chemical_formula_weight         634.83
_chemical_name_common            neivf10
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 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
;
2017-05-24 deposited with the CCDC.
2018-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.4487(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.186(2)
_cell_length_b                   13.4178(13)
_cell_length_c                   17.1643(16)
_cell_measurement_reflns_used    4019
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.57
_cell_volume                     3232.4(6)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27844
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        32.567
_diffrn_reflns_theta_max         32.567
_diffrn_reflns_theta_min         1.988
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.912
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015a)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             1327
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
; 
 Flack x determined using 3057 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.032(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         11571
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.973
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                8330
_reflns_number_total             11571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04750a2.cif
_cod_data_source_block           neivf10
_cod_depositor_comments
'Adding full bibliography for 1548638--1548640.cif.'
_cod_original_cell_volume        3232.4(7)
_cod_database_code               1548638
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.646
_shelx_estimated_absorpt_t_max   0.725
_shelx_res_checksum              33589