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_4084494
_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 O3 Ru 1+, F6 P 1-, C3 H6 O'
_chemical_formula_sum            'C34 H37 F6 O4 P Ru'
_chemical_formula_weight         755.68
_chemical_name_systematic
; 
[\h^6^-9,10-dimethoxy-4H-cyclopenta[def]triphenylene]-
[\h^5^-(hydroxymethyl)tetraamethylcyclopentadienyl]ruthenium(II) 
hexafluorophosphate  
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ntl1413
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.506(3)
_cell_angle_beta                 87.780(3)
_cell_angle_gamma                73.274(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8304(4)
_cell_length_b                   11.1390(4)
_cell_length_c                   14.5873(5)
_cell_measurement_reflns_used    12173
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.631
_cell_measurement_theta_min      4.701
_cell_volume                     1528.41(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.988
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18525
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         76.72
_diffrn_reflns_theta_min         4.70
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.321
_exptl_absorpt_correction_T_max  0.8567
_exptl_absorpt_correction_T_min  0.3173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.33.
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             772
_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          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+1.1104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                5977
_reflns_number_total             6364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5008852_si_002.cif
_cod_data_source_block           RuCpMe4CH2OH_4
_cod_depositor_comments
'Adding full bibliography for 4084487--4084494.cif.'
_cod_original_cell_volume        1528.4(1)
_cod_database_code               4084494