The influence of the ligand chelate effect on iron-amine-catalysed Kumada cross-coupling.
Bedford, Robin B.; Brenner, Peter B.; Elorriaga, David; Harvey, Jeremy N.; Nunn, Joshua; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15811–15817; doi:10.1039/c6dt01823h

data_7039569
_publ_section_title
;
 The influence of the ligand chelate effect on iron-amine-catalysed Kumada
 cross-coupling.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15811
_journal_page_last               15817
_journal_paper_doi               10.1039/c6dt01823h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C14 H32 Cl Fe N4, 3(C2 H3 N), Cl'
_chemical_formula_sum            'C20 H41 Cl2 Fe N7'
_chemical_formula_weight         506.35
_chemical_name_systematic        'C14 H32 Cl Fe N4, 3(C2 H3 N), Cl'
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-05 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                65.49(3)
_cell_angle_beta                 81.50(3)
_cell_angle_gamma                81.42(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4114(17)
_cell_length_b                   13.145(3)
_cell_length_c                   13.243(3)
_cell_measurement_reflns_used    8577
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.83
_cell_measurement_theta_min      3.67
_cell_volume                     1311.4(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Pt135 CCD area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.788
_diffrn_measured_fraction_theta_max 0.799
_diffrn_measurement_device       'Bruker Mircostar Rotating anode'
_diffrn_measurement_device_type  'Rotating anode'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.788
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8897
_diffrn_reflns_point_group_measured_fraction_full 0.788
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.864
_diffrn_reflns_theta_min         1.698
_diffrn_source                   'micro-focus rotating anode'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.3777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1286 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.5017.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0515
_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^)+3.2784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4029
_reflns_number_total             4071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01823h2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7039568--7039570.cif.'
_cod_original_cell_volume        1311.5(6)
_cod_database_code               7039569
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C42A(H42A,H42B), C41(H41A,H41B), C15(H15A,H15B), C18(H18A,H18B),
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C30(H30A,H30B)
2.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C27(H27A,H27B,H27C), C9(H9A,H9B,H9C), C11(H11A,H11B,
 H11C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'