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_4084490
_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         'C21 H16 O2'
_chemical_formula_sum            'C21 H16 O2'
_chemical_formula_weight         300.34
_chemical_name_systematic
; 
10,11-dimethoxy-4H-cyclopenta[def]triphenylene 
;
_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                ntl1402
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 113.796(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.683(5)
_cell_length_b                   10.035(5)
_cell_length_c                   13.546(5)
_cell_measurement_reflns_used    4751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.876
_cell_measurement_theta_min      4.208
_cell_volume                     1453.1(11)
_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 0.967
_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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8365
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         74.13
_diffrn_reflns_theta_min         4.23
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.9796
_exptl_absorpt_correction_T_min  0.8303
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.36.28
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             632
_exptl_crystal_preparation
;
Crystals were grown by slowly cooling a hot concentrated solution 
of the compound in ethanol to room temperature.
;
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0530P)^2^+0.3783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                2441
_reflns_number_total             2860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5008852_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4084487--4084494.cif.'
_cod_original_cell_volume        1453.1(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4084490