The crystal structure of (4E,11E,31E,38E)-1,4,12,15,18,26,31,39-Octaaza-7,21,24-trihydroxy-penta-cyclo[13·13·13·16,10·120,24·133,37]tetratetraconta-4,6(44),7,9,11,18,20(43),21,23,25,31,33(42),34,36,38-pentadecaene, C36H42N8O3
Zhang, Hui; Cao, Xin; Zhang, Bingguang; Liu, Yuhai; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 13–15; doi:10.1515/ncrs-2014-9044

data_8106771
_publ_section_title
;
 The crystal structure of
 (4E,11E,31E,38E)-1,4,12,15,18,26,31,39-Octaaza-7,21,24-trihydroxy-penta-cyclo[13&#x00B7;13&#x00B7;13&#x00B7;16,10&#x00B7;120,24&#x00B7;133,37]tetratetraconta-4,6(44),7,9,11,18,20(43),21,23,25,31,33(42),34,36,38-pentadecaene,
 C36H42N8O3
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              13
_journal_page_last               15
_journal_paper_doi               10.1515/ncrs-2014-9044
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C36 H42 N8 O3'
_chemical_formula_sum            'C36 H42 N8 O3'
_chemical_formula_weight         634.77
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   30.732(2)
_cell_length_b                   30.732(2)
_cell_length_c                   18.6315(15)
_cell_measurement_reflns_used    3209
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.394
_cell_measurement_theta_min      2.294
_cell_volume                     15239.1(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25929
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.881
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9173
_exptl_absorpt_correction_T_min  0.6112
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6084
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.00030(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.815
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         5980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.815
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2650
_reflns_number_total             5980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2014-9044_suppl.cif
_cod_data_source_block           sad
_cod_original_cell_volume        15239(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               8106771
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H2 of O2, H3 of O3, H3' of O3', All C(H,H) groups
 At 1.5 times of:
  H1 of O1
2. Others
 Fixed Sof: O2(0.33333) H2(0.3333) O2'(0.66667) H2'(0.66667) O3(0.66667)
 H3(0.66667) O3'(0.33333) H3'(0.33333)
3.a Riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
  C35(H35A,H35B), C36(H36A,H36B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C6(H6), C9(H9), C10(H10), C15(H15), C18(H18), C21(H21),
 C22(H22), C27(H27), C30(H30), C33(H33), C34(H34)
3.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O2(H2), O2'(H2'), O3(H3), O3'(H3')
;
_shelx_res_checksum              9131
_shelx_hkl_checksum              75471
_olex2_submission_special_instructions 'No special instructions were received'