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_7037773
_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         'C49 H40.115 F0.885 P2 Ru, F6 P, C H2 Cl2'
_chemical_formula_sum            'C50 H42.115 Cl2 F6.885 P3 Ru'
_chemical_formula_weight         1038.64
_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             2014-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_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                   17.5524(3)
_cell_length_b                   19.8953(4)
_cell_length_c                   25.3282(5)
_cell_measurement_reflns_used    11699
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      31.9980
_cell_measurement_theta_min      3.3790
_cell_volume                     8844.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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    'ShelXS (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 0.898
_diffrn_measurement_details
;
  1 omega  -38.00   31.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0740   77.0000   60.0000 69

  2 omega  -32.00   21.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0740   77.0000 -180.0000 53

  3 omega   29.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4802   77.0000 -120.0000 40
;
_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      -0.0293416000
_diffrn_orient_matrix_UB_12      -0.0041145000
_diffrn_orient_matrix_UB_13      0.0190323000
_diffrn_orient_matrix_UB_21      0.0170492000
_diffrn_orient_matrix_UB_22      -0.0304697000
_diffrn_orient_matrix_UB_23      0.0086093000
_diffrn_orient_matrix_UB_31      0.0219330000
_diffrn_orient_matrix_UB_32      0.0180850000
_diffrn_orient_matrix_UB_33      0.0186343000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33223
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.211
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             4216.6
_exptl_crystal_size_max          0.3926
_exptl_crystal_size_mid          0.2659
_exptl_crystal_size_min          0.1639
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         14037
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+5.1321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11505
_reflns_number_total             14037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04596g2.cif
_cod_data_source_block           '[3a]PF6_Orange_Form'
_cod_depositor_comments
'Adding full bibliography for 7037771--7037778.cif.'
_cod_database_code               7037773
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C50 H42 Cl2 F7 P3 Ru1'
_chemical_oxdiff_usercomment     LucyM-198
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F3A-F4A \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F5A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F4A)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(F3A) = Uanis(F5A)
Uanis(F6A) = Uanis(F4A)
4. Others
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(H7)=1-FVAR(2)
 Sof(F1)=FVAR(2)
 Sof(H50C)=Sof(H50D)=Sof(Cl2A)=1-FVAR(3)
 Sof(H50A)=Sof(H50B)=Sof(Cl2)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_exptl_crystal_mounting_method 'oil on loop'
_olex2_submission_special_instructions 'No special instructions were received'