Mechanistic Insight Into High-Spin Iron(I)-Catalyzed Butadiene Dimerization
Lee, Heejun; Campbell, Michael G.; Hernández Sánchez, Raúl; Börgel, Jonas; Raynaud, Jean; Parker, Sarah E.; Ritter, Tobias; Organometallics 35 (2016) 2923–; doi:10.1021/acs.organomet.6b00474

data_4088822
_publ_section_title
;
 Mechanistic Insight Into High-Spin Iron(I)-Catalyzed Butadiene
 Dimerization
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2923
_journal_paper_doi               10.1021/acs.organomet.6b00474
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C28 H36 Fe N2'
_chemical_formula_sum            'C28 H36 Fe N2'
_chemical_formula_weight         456.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_audit_creation_date             2015-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.542(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.760(1)
_cell_length_b                   13.7555(10)
_cell_length_c                   12.8368(10)
_cell_measurement_reflns_used    1650
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.19
_cell_measurement_theta_min      2.52
_cell_volume                     2408.7(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009. 3. 0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10107
_diffrn_reflns_theta_full        25.8353
_diffrn_reflns_theta_max         25.84
_diffrn_reflns_theta_min         2.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_correction_T_min  0.7719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.2586
_exptl_crystal_description       plate
_exptl_crystal_F_000             977.7021
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.5793
_refine_diff_density_min         -0.4473
_refine_diff_density_rms         0.0926
_refine_ls_d_res_high            0.8155
_refine_ls_d_res_low             9.6859
_refine_ls_goodness_of_fit_ref   0.8169
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8169
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                1601
_reflns_number_total             2324
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om6b00474_si_002.cif
_cod_data_source_block           Complex_2_isomer
_cod_database_code               4088822
_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.a Ternary CH refined with riding coordinates:
 C008(H008), C00A(H00d)
2.b Secondary CH2 refined with riding coordinates:
 C00F(H00m,H00n), C00G(H00o,H00p)
2.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00B(H00e), C00C(H00f)
2.d Idealised Me refined as rotating group:
 C007(H00a,H00b,H00c), C00D(H00g,H00h,H00i), C00E(H00j,H00k,H00l)
;
_olex2_submission_special_instructions 'No special instructions were received'