Mono-functionalized derivatives and revised configurational assignment of amide naphthotubes.
Yao, Huan; Wang, Xiaoping; Xie, Mo; Wang, Yu-Mei; Quan, Mao; Yang, Liu-Pan; Jiang, Wei; Organic & biomolecular chemistry 18 (2020) 1900–1909; doi:10.1039/d0ob00290a

data_7157362
_publ_section_title
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 Mono-functionalized derivatives and revised configurational assignment of
 amide naphthotubes.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1900
_journal_page_last               1909
_journal_paper_doi               10.1039/d0ob00290a
_journal_volume                  18
_journal_year                    2020
_chemical_formula_moiety         'C58 H42 N2 O18, 3(C4 H8 O), 2(H2 O)'
_chemical_formula_sum            'C70 H70 N2 O23'
_chemical_formula_weight         1307.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-29 deposited with the CCDC.	2020-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                80.635(2)
_cell_angle_beta                 85.048(2)
_cell_angle_gamma                74.885(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2399(5)
_cell_length_b                   15.4494(6)
_cell_length_c                   15.6625(6)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      59.07
_cell_measurement_theta_min      3.46
_cell_volume                     3048.4(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39128
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        59.229
_diffrn_reflns_theta_max         59.229
_diffrn_reflns_theta_min         2.862
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1004 before and 0.0513 after correction. The Ratio of minimum to maximum transmission is 0.8914. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         8755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0582
_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^)+(0.1069P)^2^+3.4066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7606
_reflns_number_total             8755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob00290a2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7157362--7157365.cif.'
_cod_database_code               7157362
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.775
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Sof(H53A)=Sof(H53B)=Sof(H27A)=Sof(H27B)=Sof(O22A)=Sof(O23A)=1-FVAR(1)
 Sof(H54A)=Sof(H54B)=Sof(H28A)=Sof(H28B)=Sof(O23B)=Sof(O22B)=FVAR(1)
3.a Free rotating group:
 O17(H17A,H17B)
3.b Ternary CH refined with riding coordinates:
 C67(H67), C14(H14), C69(H69), C70(H70)
3.c Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C39(H39A,H39B), C54(H54A,H54B), C28(H28A,H28B), C53(H53A,
 H53B), C27(H27A,H27B), C11(H11A,H11B), C51(H51A,H51B), C13(H13A,H13B),
 C25(H25A,H25B), C65(H65A,H65B), C61(H61A,H61B), C66(H66A,H66B), C63(H63A,H63B),
  C62(H62A,H62B), C64(H64A,H64B), C58(H58A,H58B), C60(H60A,H60B), C57(H57A,
 H57B), C55(H55A,H55B), C59(H59A,H59B), C56(H56A,H56B)
3.d Aromatic/amide H refined with riding coordinates:
 N1(H1), C47(H47), C38(H38), C37(H37), C10(H10), C44(H44), C29(H29), C1(H1A),
 C43(H43), C30(H30), C17(H17), C22(H22), C18(H18), C9(H9), C21(H21), C48(H48),
 C2(H2A)
3.e Tetrahedral OH refined with riding coordinates:
 O16(H16)
3.f Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              74441
_shelx_fab_checksum              21222
_olex2_submission_special_instructions 'No special instructions were received'