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_4124386
_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         'B F4, C37 H28 F5 N P Ru'
_chemical_formula_sum            'C37 H28 B F9 N P Ru'
_chemical_formula_weight         800.45
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.8435(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5269(2)
_cell_length_b                   12.30582(14)
_cell_length_c                   19.9237(3)
_cell_measurement_reflns_used    8993
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      28.6670
_cell_measurement_theta_min      3.4820
_cell_volume                     3257.69(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.7089
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0264734000
_diffrn_orient_matrix_UB_12      0.0495306000
_diffrn_orient_matrix_UB_13      0.0034670000
_diffrn_orient_matrix_UB_21      0.0179609000
_diffrn_orient_matrix_UB_22      -0.0184382000
_diffrn_orient_matrix_UB_23      -0.0262420000
_diffrn_orient_matrix_UB_31      -0.0427398000
_diffrn_orient_matrix_UB_32      0.0229693000
_diffrn_orient_matrix_UB_33      -0.0285498000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12746
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.2484
_exptl_crystal_size_mid          0.1618
_exptl_crystal_size_min          0.0793
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6049
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+1.5812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0510
_reflns_number_gt                5879
_reflns_number_total             6049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b06547_si_001.cif
_cod_data_source_block           jml1376
_cod_original_cell_volume        3257.69(8)
_cod_database_code               4124386
_chemical_oxdiff_formula         'C37 H28 B1 F9 N1 P1 Ru1'
_chemical_oxdiff_usercomment     LucyM-106
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
;