Bimetallic Mechanism for Alkyne Cyclotrimerization with a Two-Coordinate Fe Precatalyst
Witzke, Ryan J.; Hait, Diptarka; Chakarawet, Khetpakorn; Head-Gordon, Martin; Tilley, T. Don; ACS Catalysis  (2020) 7800–; doi:10.1021/acscatal.0c01828

data_4517830
_publ_section_title
;
 Bimetallic Mechanism for Alkyne Cyclotrimerization with a Two-Coordinate
 Fe Precatalyst
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              7800
_journal_paper_doi               10.1021/acscatal.0c01828
_journal_year                    2020
_chemical_formula_moiety         'C58 H72 Fe2 N2 Si2, 2(C7 H8)'
_chemical_formula_sum            'C72 H88 Fe2 N2 Si2'
_chemical_formula_weight         1149.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.224(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1589(9)
_cell_length_b                   20.1568(13)
_cell_length_c                   10.7730(6)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.48
_cell_volume                     3056.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30110
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.440
_diffrn_reflns_theta_min         1.447
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1128 before and 0.0774 after correction. The Ratio of minimum to maximum transmission is 0.8740. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.707
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5625
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0551P)^2^+13.1779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4325
_reflns_number_total             5625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c01828_si_003.cif
_cod_data_source_block           rjw_i_87_0ma
_cod_database_code               4517830
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C29(H29), C25(H25), C28(H28), C22(H22), C21(H21), C20(H20),
 C19(H19), C5(H5), C27(H27), C3(H3), C26(H26), C4(H4), C33(H33), C35(H35),
 C34(H34), C32(H32), C31(H31)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C), C14(H14A,H14B,
 H14C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C36(H36A,
 H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'