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_4084492
_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         'C39 H47 O2 Ru 1+, F6 P 1-, 2(C H2 Cl2)'
_chemical_formula_sum            'C41 H51 Cl4 F6 O2 P Ru'
_chemical_formula_weight         963.66
_chemical_name_systematic
; 
[\h^6^-2,6-Di(tert-butyl)-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                ntl1362
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.781(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6149(5)
_cell_length_b                   24.122(2)
_cell_length_c                   15.6796(7)
_cell_measurement_reflns_used    6508
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.800
_cell_measurement_theta_min      4.154
_cell_volume                     4183.2(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.962
_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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17039
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         75.02
_diffrn_reflns_theta_min         3.48
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.278
_exptl_absorpt_correction_T_max  0.8340
_exptl_absorpt_correction_T_min  0.2724
_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    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1976
_exptl_crystal_preparation
;
Crystals were grown by rt diffusion of ether vapour into a concentrated 
solution of the complex in dichloromethane.
;
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.109
_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     509
_refine_ls_number_reflns         8295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0673P)^2^+8.5239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                6634
_reflns_number_total             8295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5008852_si_002.cif
_cod_data_source_block           RuCpMe5_2
_cod_depositor_comments
'Adding full bibliography for 4084487--4084494.cif.'
_cod_original_cell_volume        4183.2(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4084492