10,21-Dimethyl-2,7,13,18-tetraphenyl-3,6,14,17-tetraazatricyclo[17.3.1.1^8,12^]tetracosa-1(23),2,6,8(24),9,11,13,17,19,21-decaene-23,24-diol cyclohexane 0.33-solvate
Asatkar, Ashish K.; Verma, Vinay K.; Jain, Tripti A.; Singh, Rajendra; Gupta, Sushil K.; Butcher, Ray J.; Acta Crystallographica Section E 67 (2011) o2724–o2725; doi:10.1107/S1600536811036622

data_2232071
_publ_section_title
;
 10,21-Dimethyl-2,7,13,18-tetraphenyl-3,6,14,17-tetraazatricyclo[17.3.1.1^8,12^]tetracosa-1(23),2,6,8(24),9,11,13,17,19,21-decaene-23,24-diol
 cyclohexane 0.33-solvate
;
_journal_coeditor_code           TK2788
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2724
_journal_page_last               o2725
_journal_paper_doi               10.1107/S1600536811036622
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C46 H40 N4 O2, 1/3(C6 H12)'
_chemical_formula_moiety         'C46 H40 N4 O2, 1/3(C6 H12)'
_chemical_formula_sum            'C48 H44 N4 O2'
_chemical_formula_weight         708.87
_chemical_name_systematic
;
10,21-dimethyl-2,7,13,18-tetraphenyl-3,6,14,17-
tetraazatricyclo[17.3.1.1^8,12^]tetracosa-1(23),2,6,8(24),9,11,13,17,19,21-
decaene-23,24-diol cyclohexane 0.33-solvate
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   28.0966(2)
_cell_length_b                   28.0966(2)
_cell_length_c                   16.0265(2)
_cell_measurement_reflns_used    3689
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      77.3830
_cell_measurement_theta_min      4.1777
_cell_volume                     10956.63(18)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10270
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.32
_platon_squeeze_details
;
;
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0631
_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^)+(0.1584P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2215
_reflns_number_gt                3022
_reflns_number_total             5016
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2788.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2017-04-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        10956.6(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_moiety     '3(C46 H40 N4 O2), C6 H12'
_cod_original_formula_sum        'C144 H132 N12 O6'
_cod_original_formula_units_Z    3
_cod_original_formula_weight     2126.62
_cod_database_code               2232071
_cod_database_fobs_code          2232071