Synthesis of (μ<sup>2</sup>,η<sup>3</sup>-allyl-η<sup>5</sup>-oxapentadienyl)diiron pentacarbonyl complexes, an unusual reaction product from η<sup>4</sup>-(vinylketene)Fe(CO)<sub>3</sub> complexes: structure and electron density distribution analysis.
Resendiz-Lara, Diego A; Rosas-Sánchez, Alfredo; Hashizume, Daisuke; Barquera-Lozada, José E; Toscano, R. Alfredo; López-Cortés, José G; Ortega-Alfaro, M Carmen; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2722–2734; doi:10.1039/d2dt03700a

data_7712203
_publ_section_title
;
 Synthesis of
 (&#x3bc;<sup>2</sup>,&#x3b7;<sup>3</sup>-allyl-&#x3b7;<sup>5</sup>-oxapentadienyl)diiron
 pentacarbonyl complexes, an unusual reaction product from
 &#x3b7;<sup>4</sup>-(vinylketene)Fe(CO)<sub>3</sub> complexes: structure
 and electron density distribution analysis.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2722
_journal_page_last               2734
_journal_paper_doi               10.1039/d2dt03700a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C24 H18 Fe2 O4, 0.25(C H2 Cl2)'
_chemical_formula_sum            'C24.25 H18.5 Cl0.5 Fe2 O4'
_chemical_formula_weight         503.31
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2023-01-25 deposited with the CCDC.	2023-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.8530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2932(8)
_cell_length_b                   11.1212(6)
_cell_length_c                   13.2838(7)
_cell_measurement_reflns_used    5618
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.26
_cell_volume                     2277.9(2)
_computing_cell_refinement       'APEX3 v2019.1-0(Bruker, 2019)'
_computing_data_collection       'APEX3 v2019.1-0(Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2014)'
_computing_molecular_graphics    'SHELXLe (H\"ubschle et al, 2011)'
_computing_publication_material  'CIFTAB V 2013/2 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2012 (Bruker, 2013)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker Smart Apex CCD diffractometer 01-670-01'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18422
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.339
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       lamina
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.074
_platon_squeeze_details
;
The presence of CH2Cl2 solvent molecules used in the re-crystallization 
could be seen by the residual peaks located in the open channels around 
the  Wyckoff positions b (0.500  0.000  0.000 and 0.500  0.500  0.500). 
Unfortunately, they were statistically and orientationally disordered so 
badly that it could not be modeled even with restraints. Consequently, 
SQUEEZE (from PLATON:A. L. Spek, Acta Cryst. 2015, C71, 9) was used to 
calculate the void space, the electron count and to get a new HKL file. 
According to the SQUEEZE results, a total number of 1 CH2Cl2 
(42 electrons) was considered per unit cell. All parameters reported in 
the CIF take the solvent molecules into account, leading to 
FORMU01_ALERT_2, CELLZ01_ALERT_1 and PLAT051_ALERT_1 alerts in the 
checkCIF report
;
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4143
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0673P)^2^+0.1631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2741
_reflns_number_total             4143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03700a2.cif
_cod_data_source_block           Compound_3b_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7712202--7712205.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C24.25 H18.50 Cl0.50 Fe2 O4'
_cod_database_code               7712203
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.655
_shelx_estimated_absorpt_t_max   0.906
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              44245
_shelx_fab_checksum              10832