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_4084493
_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         'C31 H31 O2 Ru 1+, F6 P 1-'
_chemical_formula_sum            'C31 H31 F6 O2 P Ru'
_chemical_formula_weight         681.60
_chemical_name_systematic
; 
[\h^6^-9,10-dimethoxy-4H-cyclopenta[def]triphenylene]-
(\h^5^-pentamethylcyclopentadienyl)ruthenium(II) hexafluorophosphate  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ntl1411
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.560(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9764(1)
_cell_length_b                   13.6695(3)
_cell_length_c                   22.4179(4)
_cell_measurement_reflns_used    11858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.052
_cell_measurement_theta_min      3.777
_cell_volume                     2726.83(8)
_computing_cell_refinement       'CrysAlisPro (Agilent, V 1.171.37.33)'
_computing_data_collection       'CrysAlisPro (Agilent, V 1.171.37.33)'
_computing_data_reduction        'CrysAlisPro (Agilent, V 1.171.37.33)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.970
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15481
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         74.12
_diffrn_reflns_theta_min         3.80
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.836
_exptl_absorpt_correction_T_max  0.5930
_exptl_absorpt_correction_T_min  0.3882
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.33.
Numerical absorption correction based on gaussian integration over 
a multifaceted crystal model. Empirical absorption correction using 
spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_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          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0366P)^2^+2.0280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                5126
_reflns_number_total             5378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5008852_si_002.cif
_cod_data_source_block           RuCpMe5_4
_cod_depositor_comments
'Adding full bibliography for 4084487--4084494.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4084493