Outer-Sphere Electrophilic Fluorination of Organometallic Complexes.
Milner, Lucy M.; Pridmore, Natalie E.; Whitwood, Adrian C.; Lynam, Jason M.; Slattery, John M.; Journal of the American Chemical Society 137 (2015) 10753–10759; doi:10.1021/jacs.5b06547

data_4124387
_publ_section_title
;
 Outer-Sphere Electrophilic Fluorination of Organometallic Complexes.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10753
_journal_page_last               10759
_journal_paper_doi               10.1021/jacs.5b06547
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C37 H29 F4 N P Ru, B F4'
_chemical_formula_sum            'C37 H29 B F8 N P Ru'
_chemical_formula_weight         782.46
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.9459(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.34095(17)
_cell_length_b                   17.7554(3)
_cell_length_c                   9.85967(18)
_cell_measurement_reflns_used    11823
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      32.0350
_cell_measurement_theta_min      3.3940
_cell_volume                     1593.68(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_temperature      110.05(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0563344000
_diffrn_orient_matrix_UB_12      0.0089598000
_diffrn_orient_matrix_UB_13      0.0589554000
_diffrn_orient_matrix_UB_21      -0.0379956000
_diffrn_orient_matrix_UB_22      -0.0201217000
_diffrn_orient_matrix_UB_23      0.0432125000
_diffrn_orient_matrix_UB_31      0.0381281000
_diffrn_orient_matrix_UB_32      -0.0333183000
_diffrn_orient_matrix_UB_33      -0.0103150000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20566
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         32.33
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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)
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.1405
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.028(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         10120
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.2436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                9603
_reflns_number_total             10120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b06547_si_002.cif
_cod_data_source_block           jml1390
_cod_database_code               4124387
_chemical_oxdiff_formula         'C37 H29 B1 F8 N1 P1 Ru1'
_chemical_oxdiff_usercomment     'Lucy's LucyM-107'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
;