Iron(ii)-induced cycloisomerization of alkynes via"non-vinylidene" pathways for iron(ii)-indolizine and -indolizinone complexes.
Chan, Siu-Chung; Yeung, Chi-Fung; Shek, Hau-Lam; Ng, Sze-Wing; Tse, Sheung-Ying; Tse, Man-Kit; Yiu, Shek-Man; Wong, Chun-Yuen; Chemical communications (Cambridge, England) 56 (2020) 12644–12647; doi:10.1039/d0cc05081d

data_7127322
_publ_section_title
;
 Iron(ii)-induced cycloisomerization of alkynes
 via&quot;non-vinylidene&quot; pathways for iron(ii)-indolizine and
 -indolizinone complexes.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12644
_journal_page_last               12647
_journal_paper_doi               10.1039/d0cc05081d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C20 H20 F6 Fe N2 O7 S5'
_chemical_formula_weight         730.53
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-07-21 deposited with the CCDC.	2020-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.7380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.4848(7)
_cell_length_b                   11.4726(3)
_cell_length_c                   20.4806(6)
_cell_measurement_reflns_used    8828
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      74.41
_cell_measurement_theta_min      4.30
_cell_volume                     5448.2(3)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Apex3'
_computing_data_reduction        'Bruker Saint'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24565
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.466
_diffrn_reflns_theta_min         3.813
_diffrn_source                   'micro focus'
_exptl_absorpt_coefficient_mu    8.828
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5543
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0595
_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^)+(0.1081P)^2^+0.2861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4312
_reflns_number_total             5543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05081d2.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
'Adding full bibliography for 7127322--7127325.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7127322
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              83215
_shelx_hkl_checksum              55014