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_7037776
_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         'C55 H43 F3 N P2 Ru, B F4, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C55.5 H44 B Cl F7 N P2 Ru'
_chemical_formula_weight         1067.18
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-08-20 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.805(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3433(2)
_cell_length_b                   23.9394(5)
_cell_length_c                   19.3083(4)
_cell_measurement_reflns_used    4462
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      27.7210
_cell_measurement_theta_min      4.1490
_cell_volume                     4724.63(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_details
;
  1 omega   -6.00   83.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3846   57.0000   30.0000 89

  2 omega  -45.00   39.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3846  -77.0000  -90.0000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Supernova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0096849000
_diffrn_orient_matrix_UB_12      0.0163035000
_diffrn_orient_matrix_UB_13      -0.0310521000
_diffrn_orient_matrix_UB_21      0.0054347000
_diffrn_orient_matrix_UB_22      -0.0243659000
_diffrn_orient_matrix_UB_23      -0.0202659000
_diffrn_orient_matrix_UB_31      -0.0684577000
_diffrn_orient_matrix_UB_32      -0.0042526000
_diffrn_orient_matrix_UB_33      -0.0029623000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_laue_measured_fraction_full 0.983
_diffrn_reflns_laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15633
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.011
_diffrn_reflns_theta_min         3.505
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       needle
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.3297
_exptl_crystal_size_mid          0.0526
_exptl_crystal_size_min          0.0173
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0249P)^2^+2.8424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0862
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7108
_reflns_number_total             9356
_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_original_cell_volume        4724.64(17)
_cod_original_formula_sum        'C55.50 H44 B Cl F7 N P2 Ru'
_cod_database_code               7037776
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C55.5 H44 B1 F4 N1 O1 P2 Ru1 Cl1'
_chemical_oxdiff_usercomment     LucyM-339/340
_reflns_odcompleteness_completeness 93.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 C19-F1 \\sim C19-F2 \\sim C19-F3A \\sim C19-F3 \\sim C19-F2A \\sim C19-F1
\\sim C19-F1A
 with sigma of 0.02
 F1-F2 \\sim F1A-F2A \\sim F2-F3 \\sim F2A-F3A \\sim F3-F1 \\sim F3A-F1A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F2) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F2A) = Uanis(F2)
Uanis(F3A) = Uanis(F3)
Uanis(F1) = Uanis(F1A)
3. Others
 Sof(F1)=Sof(F2)=Sof(F3)=1-FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(F1A)=FVAR(1)
 Fixed Sof: C56(0.5) H56a(0.5) H56b(0.5) Cl1(0.5) Cl2(0.5)
;
_olex2_date_sample_data_collection 2014-12-11
_olex2_date_sample_submission    2014-12-08
_olex2_exptl_crystal_mounting_method 'oil on loop'
_olex2_submission_special_instructions 'No special instructions were received'