Access to novel fluorovinylidene ligands via exploitation of outer-sphere electrophilic fluorination: new insights into C-F bond formation and activation.
Milner, Lucy M.; Hall, Lewis M.; Pridmore, Natalie E.; Skeats, Matthew K.; Whitwood, Adrian C.; Lynam, Jason M.; Slattery, John M.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1717–1726; doi:10.1039/c5dt04596g

data_7037774
_publ_section_title
;
 Access to novel fluorovinylidene ligands via exploitation of outer-sphere
 electrophilic fluorination: new insights into C-F bond formation and
 activation.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1717
_journal_page_last               1726
_journal_paper_doi               10.1039/c5dt04596g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C50 H40 F3 P2 Ru, C H2 Cl2, B F4'
_chemical_formula_sum            'C51 H42 B Cl2 F7 P2 Ru'
_chemical_formula_weight         1032.56
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-12-19 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8473(4)
_cell_length_b                   14.6795(3)
_cell_length_c                   35.2252(16)
_cell_measurement_reflns_used    10017
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      31.8300
_cell_measurement_theta_min      3.1760
_cell_volume                     9228.6(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0112153000
_diffrn_orient_matrix_UB_12      0.0412558000
_diffrn_orient_matrix_UB_13      0.0088243000
_diffrn_orient_matrix_UB_21      -0.0206736000
_diffrn_orient_matrix_UB_22      0.0119677000
_diffrn_orient_matrix_UB_23      -0.0164607000
_diffrn_orient_matrix_UB_31      -0.0320249000
_diffrn_orient_matrix_UB_32      -0.0221586000
_diffrn_orient_matrix_UB_33      0.0075219000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            28548
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.036
_diffrn_reflns_theta_min         2.911
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.989
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.2616
_exptl_crystal_size_mid          0.1943
_exptl_crystal_size_min          0.1582
_refine_diff_density_max         1.140
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         13431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0117P)^2^+12.2802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11009
_reflns_number_total             13431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04596g2.cif
_cod_data_source_block           '[5a]BF4'
_cod_depositor_comments
'Adding full bibliography for 7037771--7037778.cif.'
_cod_database_code               7037774
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C50 H40 F7 B1 P2 Ru1'
_chemical_oxdiff_usercomment     LucyM-164
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl2) = Uanis(Cl2A)
Uanis(F5) = Uanis(F6A)
Uanis(F5A) = Uanis(F7)
3. Others
 Sof(H51C)=Sof(H51D)=Sof(Cl2A)=1-FVAR(1)
 Sof(H51A)=Sof(H51B)=Sof(Cl2)=FVAR(1)
 Sof(F5A)=Sof(F6A)=Sof(F7A)=1-FVAR(2)
 Sof(F5)=Sof(F6)=Sof(F7)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C51(H51C,H51D)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50)
;
_shelx_res_checksum              57850