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_7039570
_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         'C21 H21 Fe, 1.5(C7 H8), C18 H48 Cl5 Mg3 N6'
_chemical_formula_sum            'C49.5 H81 Cl5 Fe Mg3 N6'
_chemical_formula_weight         1066.23
_chemical_name_systematic        'C21 H21 Fe, 1.5(C7 H8), C18 H48 Cl5 Mg3 N6'
_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
_audit_creation_date             2016-05-05
_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                90
_cell_angle_beta                 101.622(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0139(19)
_cell_length_b                   18.539(2)
_cell_length_c                   21.231(3)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      26.59
_cell_volume                     5788.3(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Pt135 CCD area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.759
_diffrn_measured_fraction_theta_max 0.773
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.759
_diffrn_reflns_Laue_measured_fraction_max 0.773
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20844
_diffrn_reflns_point_group_measured_fraction_full 0.759
_diffrn_reflns_point_group_measured_fraction_max 0.773
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.788
_diffrn_reflns_theta_min         26.495
_diffrn_source                   'micro-focus rotating anode'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.808
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.2876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         7944
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0864P)^2^+5.1262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6932
_reflns_number_total             7944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01823h2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7039568--7039570.cif.'
_cod_original_cell_volume        5788.3(12)
_cod_original_formula_sum        'C49.50 H81 Cl5 Fe Mg3 N6'
_cod_database_code               7039570
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Fixed Sof: C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C47(0.5) C48(0.5) H48(0.5)
 C49(0.5) H49(0.5) C50(0.5) H50(0.5) C51(0.5) H51(0.5) C52(0.5) H52(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C19(H19A,H19B), C26(H26A,H26B), C9(H9A,H9B), C10(H10A,H10B),
 C16(H16A,H16B), C4(H4A,H4B), C3(H3A,H3B), C15(H15A,H15B)
4.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C35(H35), C32(H32), C36(H36), C28(H28), C25(H25), C37(H37),
 C38(H38), C30(H30), C31(H31), C21(H21), C22(H22), C24(H24), C29(H29), C23(H23),
  C44(H44), C42(H42), C41(H41), C45(H45), C43(H43), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52)
4.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C),
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C),
 C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C),
 C17(H17A,H17B,H17C), C46(H46A,H46B,H46C)
;
_olex2_submission_special_instructions 'No special instructions were received'