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_1568619
_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 B F Mo N6 O2'
_chemical_formula_sum            'C18 H22 B F Mo N6 O2'
_chemical_formula_weight         480.16
_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
_audit_creation_date             2022-12-05
_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                 96.493(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9256(3)
_cell_length_b                   13.8329(7)
_cell_length_c                   19.1940(9)
_cell_measurement_reflns_used    9328
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.5430
_cell_measurement_theta_min      3.5370
_cell_volume                     2090.82(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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 0.997
_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    -19.00   7.00   1.00   42.80    --  -11.30 -77.00  60.00   26
  2  \w    -14.00  13.00   1.00   42.80    --  -11.30 -99.00   0.00   27
  3  \w     40.00  89.00   1.00   42.80    --   11.61 178.00 -30.00   49
  4  \w    -13.00  81.00   1.00   42.80    --   11.61  37.00  30.00   94
  5  \w    -20.00  34.00   1.00   42.80    --   11.61  77.00-150.00   54
  6  \w    -11.00  86.00   1.00   42.80    --   11.61  37.00 120.00   97
;
_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      0.0199339000
_diffrn_orient_matrix_UB_12      0.0050270000
_diffrn_orient_matrix_UB_13      0.0367866000
_diffrn_orient_matrix_UB_21      0.0067153000
_diffrn_orient_matrix_UB_22      0.0507825000
_diffrn_orient_matrix_UB_23      -0.0040192000
_diffrn_orient_matrix_UB_31      -0.0875777000
_diffrn_orient_matrix_UB_32      0.0050384000
_diffrn_orient_matrix_UB_33      0.0037541000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4958
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.260
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_recrystallization_method
'Grown from the evaporation of a acetonitrole, benzene, chloroform, dichloromethane, ethanol, tetrahydrofuran solvent mixture.'
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.671
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4958
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0492P)^2^+10.5732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4423
_reflns_number_total             4958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00261f3.cif
_cod_data_source_block           rm-075-2022red_twin1
_cod_depositor_comments
'Adding full bibliography for 1568618--1568619.cif.'
_cod_database_code               1568619
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H22 B F N6 O2 Mo'
_chemical_oxdiff_usercomment     'Evap of many solvents'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.764
_reflns_odcompleteness_completeness 89.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8528(11)
 0.1472(11)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C17-C14
 1.5 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C17) = Uanis(C12)
5.a Ternary CH refined with riding coordinates:
 B1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C15(H15)
5.c 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              27422
_shelx_hkl_checksum              72162
_ins_header
;
TITL rm-075-2022red_twin1 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073   7.925640  13.832919  19.194048  90.0000  96.4930  90.0000
ZERR    4.00   0.000332   0.000714   0.000871   0.0000   0.0040   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O F Mo
UNIT 72.00 88.00 4.00 24.00 8.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.04 0.29 0.43
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id '[Mo(CF)(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 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.872