Selective para-Halogenation and Dimerization of N,C,N'-Arylruthenium(II) and -(III) 2,2':6',2''-Terpyridine Cations
Sipke H. Wadman; Remco W. A. Havenith; Martin Lutz; Anthony L. Spek; Gerard P. M. van Klink; Gerard van Koten; Journal of the American Chemical Society 132 (2010) 1914–1924; doi:10.1021/ja9073276

data_4101876
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 Selective para-Halogenation and Dimerization of N,C,N'-Arylruthenium(II)
 and -(III) 2,2':6',2''-Terpyridine Cations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1914
_journal_page_last               1924
_journal_paper_doi               10.1021/ja9073276
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C27 H29 Cl N5 Ru, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C29 H32 Cl F12 N6 P2 Ru'
_chemical_formula_weight         891.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            48
_cell_length_a                   47.7085(2)
_cell_length_b                   81.9437(4)
_cell_length_c                   10.5045(1)
_cell_measurement_reflns_used    230370
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     41066.4(5)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'HKL2000, Sortav'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       106
_diffrn_reflns_limit_k_min       -103
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            129442
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sortav
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             21456
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.034(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         23323
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+3.9012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                20026
_reflns_number_total             23323
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9073276_si_001.cif
_cod_data_source_block           s3805a
_cod_database_code               4101876