Crystal structure of tricarbon-yl[η<sup>4</sup>-6-<i>exo</i>-(tri-phenyl-phosphino)cyclo-hepta-2,4-dien-1-one]iron(0) tetra-fluoro-borate.
Wong, Kelsey C.; Reinheimer, Eric W.; Nataro, Chip; Griffith, Daniel R.; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 746–750; doi:10.1107/S2056989024005747

data_2023166
_publ_section_title
;
 Crystal structure of
 tricarbon-yl[&#x3b7;<sup>4</sup>-6-<i>exo</i>-(tri-phenyl-phosphino)cyclo-hepta-2,4-dien-1-one]iron(0)
 tetra-fluoro-borate.
;
_journal_coeditor_code           VU2002
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              746
_journal_page_last               750
_journal_paper_doi               10.1107/S2056989024005747
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Fe (C28 H22 O4) (C O)3] B F4, 0.5C H2 Cl2'
_chemical_formula_moiety         '2(C28 H22 Fe O4 P +), 2(B F4 -), C H2 Cl2'
_chemical_formula_sum            'C28.5 H23 B Cl F4 Fe O4 P'
_chemical_formula_weight         638.5701
_chemical_name_systematic
;
Tricarbonyl[\h^4^-6-<i>exo</i>-(triphenylphosphino)cyclohepta-2,4-dien-1-one]\
iron(0) tetrafluoroborate dichloromethane hemisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                86.993(2)
_cell_angle_beta                 82.468(2)
_cell_angle_gamma                77.300(2)
_cell_formula_units_Z            4
_cell_length_a                   9.9343(2)
_cell_length_b                   10.9767(3)
_cell_length_c                   26.4168(6)
_cell_measurement_reflns_used    14608
_cell_measurement_temperature    99.96(18)
_cell_measurement_theta_max      25.9240
_cell_measurement_theta_min      2.3160
_cell_volume                     2785.09(12)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
Olex2 1.3-ac4 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.3-ac4 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i>  (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      99.96(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            59046
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         2.038
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.430
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         9882
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0554P)^2^+0.9998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                7785
_reflns_number_total             9882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vu2002.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023166.cif.'
_cod_original_formula_sum        'C28.50 H23 B Cl F4 Fe O4 P'
_cod_database_code               2023166
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.942
_shelx_hkl_checksum              70236
_shelx_res_checksum              50110