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_7037777
_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         'C54 H45 F N P2 Ru, B F4'
_chemical_formula_sum            'C54 H45 B F5 N P2 Ru'
_chemical_formula_weight         976.73
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2015-08-20 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                72.589(5)
_cell_angle_beta                 89.929(4)
_cell_angle_gamma                79.010(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6304(5)
_cell_length_b                   13.5851(7)
_cell_length_c                   15.1453(9)
_cell_measurement_reflns_used    8373
_cell_measurement_temperature    109.8(6)
_cell_measurement_theta_max      31.4280
_cell_measurement_theta_min      3.2450
_cell_volume                     2237.5(2)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109.8(6)
_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 0.879
_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      0.0249400000
_diffrn_orient_matrix_UB_12      -0.0168649000
_diffrn_orient_matrix_UB_13      0.0460771000
_diffrn_orient_matrix_UB_21      -0.0525579000
_diffrn_orient_matrix_UB_22      -0.0161590000
_diffrn_orient_matrix_UB_23      0.0166543000
_diffrn_orient_matrix_UB_31      0.0221143000
_diffrn_orient_matrix_UB_32      -0.0507205000
_diffrn_orient_matrix_UB_33      -0.0041398000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71071
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20403
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         31.803
_diffrn_reflns_theta_min         3.083
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.941
_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    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.1731
_exptl_crystal_size_mid          0.1338
_exptl_crystal_size_min          0.0366
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         13479
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0286P)^2^+0.8860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11370
_reflns_number_total             13479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04596g2.cif
_cod_data_source_block           '[11]BF4'
_cod_depositor_comments
'Adding full bibliography for 7037771--7037778.cif.'
_cod_database_code               7037777
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C54 H45 F5 P2 N1 B1 Ru1'
_chemical_oxdiff_usercomment     LUCYM-171
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 B1A-F4 = B1A-F2 = B1A-F3 = B1A-F5
 1.4 with sigma of 0.02
 B1A-F4A = B1A-F2A = B1A-F3A = B1A-F5A
 1.4 with sigma of 0.02
 F4-F2 = F4-F3 = F4-F5
 2.285 with sigma of 0.04
 F2-F3 = F2-F5 = F3-F5
 2.285 with sigma of 0.04
 F4A-F2A = F4A-F3A = F4A-F5A
 2.285 with sigma of 0.04
 F2A-F3A = F2A-F5A = F3A-F5A
 2.285 with sigma of 0.04
2. Others
 Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=FVAR(1)
;