Site Selectivity of [RuCp*]+Complexation in Cyclopenta[def]triphenylenes
Hoggard, Bryce R.; Larsen, Christopher B.; Lucas, Nigel T.; Organometallics 33 (2014) 6200–; doi:10.1021/om5008852

data_4084491
_publ_section_title
;
 Site Selectivity of [RuCp*]+Complexation in Cyclopenta[def]triphenylenes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6200
_journal_paper_doi               10.1021/om5008852
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
'0.7(C29 H27 Ru 1+), 0.3(C29 H27 Ru 1+), F6 P 1+, C1.5 H3 O0.5'
_chemical_formula_sum            'C30.5 H30 F6 O0.5 P Ru'
_chemical_formula_weight         650.58
_chemical_name_systematic
; 
(\h^6^-4H-cyclopenta[def]triphenylene)-
(\h^5^-pentaamethylcyclopentadienyl)ruthenium(II) hexafluorophosphate  
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ntl1369
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.021(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.8046(3)
_cell_length_b                   12.8374(3)
_cell_length_c                   30.8461(7)
_cell_measurement_reflns_used    8657
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.539
_cell_measurement_theta_min      4.726
_cell_volume                     5398.8(2)
_computing_cell_refinement       'CrysAlisPro (Agilent, V 1.171.36.28)'
_computing_data_collection       'CrysAlisPro (Agilent, V 1.171.36.28)'
_computing_data_reduction        'CrysAlisPro (Agilent, V 1.171.36.28)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'enCIFer (CCDC, 2014)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_crystal_treatment
; 
Crystal was attached with Paratone N oil to a 0.3 mm CryoLoop supported 
in a copper mounting pin, then quenched in a cold nitrogen gas from a gas
stream from an Oxford Cryosystems Cryostream.
;
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            17397
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         76.62
_diffrn_reflns_theta_min         4.73
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.821
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.36.28.
Numerical absorption correction based on gaussian integration over 
a multifaceted crystal model
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2640
_exptl_crystal_preparation
;
Crystals were grown by rt diffusion of ether vapour into a concentrated 
solution of the complex in acetone.
;
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         5606
_refine_ls_number_restraints     485
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1268P)^2^+11.8422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.1930
_reflns_number_gt                4754
_reflns_number_total             5606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5008852_si_002.cif
_cod_data_source_block           RuCpMe5_1
_cod_depositor_comments
'Adding full bibliography for 4084487--4084494.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4084491