Enantiomorphs of a carbene‒ruthenium(II)‒porphyrin complex with four `chiral pillars'
Hirasawa, Kai; Yuge, Hidetaka; Miyamoto, Takeshi Ken; Acta Crystallographica Section C 64 (2008) m97–m100; doi:10.1107/S0108270107068059

data_2016444
_publ_section_title
;
 Enantiomorphs of a carbene--ruthenium(II)--porphyrin complex with four
 `chiral pillars'
;
_journal_coeditor_code           LN3081
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m97
_journal_page_last               m100
_journal_paper_doi               10.1107/S0108270107068059
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'[Ru (C84 H76 N4) (C15 H10 O2) (C2 H6 O)], 2C2 H6 O, 2C H2 Cl2'
_chemical_formula_moiety
;
C101 H92 N4 O3 Ru, 2(C2 H6 O), 2(C H2 Cl2)
;
_chemical_formula_sum            'C107 H108 Cl4 N4 O5 Ru'
_chemical_formula_weight         1772.85
_chemical_name_systematic
;
(dibenzoylmethylene-\k<i>C</i>)(ethanol-\k<i>O</i>)[5,10,15,20-tetrakis-\
{(1<i>R</i>,4<i>S</i>,5<i>S</i>,8<i>R</i>)-1,2,3,4,5,6,7,8-octahydro-1,4:5,\
8-dimethanoanthracen-9-yl}porphyrinato-\k^4^<i>N</i>]ruthenium(II)
dichloromethane disolvate ethanol disolvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7694(15)
_cell_length_b                   23.691(3)
_cell_length_c                   26.794(3)
_cell_measurement_reflns_used    24297
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      27.4834
_cell_measurement_theta_min      3.041
_cell_volume                     8740.5(18)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120.0(10)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68786
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.9378
_exptl_absorpt_correction_T_min  0.8907
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(NUMABS; Rigaku, 2005)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.978
_refine_ls_abs_structure_details 'Flack (1983), 9149 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.046(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1095
_refine_ls_number_reflns         20000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+7.1373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                18189
_reflns_number_total             20000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ln3081.cif
_cod_data_source_block           II
_cod_database_code               2016444
_cod_database_fobs_code          2016444