Fluorocarbyne complexes <i>via</i> electrophilic fluorination of carbido ligands.
Manzano, Richard A.; Hill, Anthony F.; Chemical science 14 (2023) 3776–3781; doi:10.1039/d3sc00261f

data_1568618
_publ_section_title
;
 Fluorocarbyne complexes <i>via</i> electrophilic fluorination of carbido
 ligands.
;
_journal_issue                   14
_journal_name_full               'Chemical science'
_journal_page_first              3776
_journal_page_last               3781
_journal_paper_doi               10.1039/d3sc00261f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C18 H22 Au B Cl F N6 O2 W'
_chemical_formula_sum            'C18 H22 Au B Cl F N6 O2 W'
_chemical_formula_weight         800.49
_chemical_name_systematic        W(u-CF)(AuCl)(CO)2(Tp*)
_chemical_properties_physical    Air-sensitive,Heat-sensitive,Light-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-24
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-15 deposited with the CCDC.	2023-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.744(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6629(9)
_cell_length_b                   10.2338(5)
_cell_length_c                   20.6113(12)
_cell_measurement_reflns_used    5144
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.2450
_cell_measurement_theta_min      3.9740
_cell_volume                     2367.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -8.00 49.00 1.00 187.50 -- 11.61 37.00 60.00 57 2 \w -37.00 82.00 1.00 187.50 -- 11.61 0.00 0.00 119'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0609216000
_diffrn_orient_matrix_UB_12      -0.0179674000
_diffrn_orient_matrix_UB_13      -0.0070012000
_diffrn_orient_matrix_UB_21      0.0138662000
_diffrn_orient_matrix_UB_22      -0.0427633000
_diffrn_orient_matrix_UB_23      0.0281367000
_diffrn_orient_matrix_UB_31      -0.0097368000
_diffrn_orient_matrix_UB_32      0.0514622000
_diffrn_orient_matrix_UB_33      0.0209001000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10721
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.630
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.190
_exptl_absorpt_correction_T_max  0.61248
_exptl_absorpt_correction_T_min  0.60550
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
'CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020) Spherical absorption correction using equivalent radius and absorption coefficient. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.246
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.048
_exptl_crystal_size_rad          0.053
_refine_diff_density_max         1.972
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0282P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3942
_reflns_number_total             4839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00261f3.cif
_cod_data_source_block           rm-069-2022bred
_cod_depositor_comments
'Adding full bibliography for 1568618--1568619.cif.'
_cod_database_code               1568618
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H22 Au B Cl F N6 O2'
_chemical_oxdiff_usercomment
'Grown from slow evaporation of a dcm hexane solution'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C15(H15)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              72734
_shelx_hkl_checksum              7902
_ins_header
'TITL rm-069-2022bred in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 11.662949 10.233835 20.611280 90.0000 105.7440 90.0000 ZERR 4.00 0.000858 0.000513 0.001194 0.0000 0.0067 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H B N O F Cl Au UNIT 72.00 88.00 4.00 24.00 8.00 4.00 4.00 4.00 TREF HKLF 4 END'
_measurement_temperature         150
_olex2_submission_original_sample_id W(u-CF)(AuCl)(CO)2(Tp*)
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
'Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling'
_oxdiff_exptl_absorpt_empirical_full_max 2.096
_oxdiff_exptl_absorpt_empirical_full_min 0.772