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_7037778
_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         'C41 H34 N2 P Ru, 0.5(C5 H5 N), B F4'
_chemical_formula_sum            'C43.5 H36.5 B F4 N2.5 P Ru'
_chemical_formula_weight         813.10
_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     direct
_audit_creation_date             2014-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-08-20 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                99.508(4)
_cell_angle_beta                 101.789(6)
_cell_angle_gamma                90.366(5)
_cell_formula_units_Z            4
_cell_length_a                   9.6081(8)
_cell_length_b                   17.9440(7)
_cell_length_c                   21.3274(10)
_cell_measurement_reflns_used    3281
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      28.0980
_cell_measurement_theta_min      6.2440
_cell_volume                     3546.9(4)
_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    '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 0.853
_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      0.0105579000
_diffrn_orient_matrix_UB_12      -0.0130587000
_diffrn_orient_matrix_UB_13      -0.0319267000
_diffrn_orient_matrix_UB_21      -0.0742194000
_diffrn_orient_matrix_UB_22      -0.0078222000
_diffrn_orient_matrix_UB_23      -0.0109128000
_diffrn_orient_matrix_UB_31      -0.0085232000
_diffrn_orient_matrix_UB_32      0.0371576000
_diffrn_orient_matrix_UB_33      -0.0071947000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16538
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.326
_diffrn_reflns_theta_min         2.915
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   analytical
_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)
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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       plate
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.4117
_exptl_crystal_size_mid          0.2117
_exptl_crystal_size_min          0.0261
_refine_diff_density_max         1.345
_refine_diff_density_min         -2.026
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         16538
_refine_ls_number_restraints     636
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0988P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10765
_reflns_number_total             16538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04596g2.cif
_cod_data_source_block           '[12]BF4.py'
_cod_depositor_comments
'Adding full bibliography for 7037771--7037778.cif.'
_cod_original_cell_volume        3547.0(4)
_cod_original_formula_sum        'C43.50 H36.50 B F4 N2.50 P Ru'
_cod_database_code               7037778
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C43.5 H36.5 B1 F4 N2.5 P1 Ru1'
_chemical_oxdiff_usercomment     'Lucym-171 red plate'
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.005 and
sigma for terminal atoms of 0.01
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_exptl_crystal_mounting_method 'oil on loop'