Mechanistic insight into ruthenium catalysed meta-sulfonation of 2-phenylpyridine
Marcé, Patricia; Paterson, Andrew J.; Mahon, Mary F.; Frost, Christopher G.; Catal. Sci. Technol. 6 (2016) 7068–; doi:10.1039/C6CY01254J

data_1543573
_publ_section_title
;
 Mechanistic insight into ruthenium catalysed meta-sulfonation of
 2-phenylpyridine
;
_journal_issue                   19
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              7068
_journal_paper_doi               10.1039/C6CY01254J
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C26 H26 N5 O2 Ru S, F6 P, C4 H10 O'
_chemical_formula_sum            'C30 H36 F6 N5 O3 P Ru S'
_chemical_formula_weight         792.74
_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     iterative
_audit_creation_date             2016-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-13 deposited with the CCDC.
2016-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                95.0620(10)
_cell_angle_beta                 92.8540(10)
_cell_angle_gamma                97.4490(10)
_cell_formula_units_Z            2
_cell_length_a                   8.28700(10)
_cell_length_b                   8.48600(10)
_cell_length_c                   25.3050(5)
_cell_measurement_reflns_used    55047
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1754.25(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29703
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.652
_diffrn_reflns_theta_min         3.581
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7976
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0327P)^2^+1.0222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6335
_reflns_number_total             7976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cy01254j2.cif
_cod_data_source_block           k13cgf2
_cod_depositor_comments          'Adding full bibliography for 1543573.cif.'
_cod_database_code               1543573
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.835
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'