Folding-Generated Molecular Tubes Containing One-Dimensional Water Chains.
Jeon, Hae-Geun; Jung, Jin Young; Kang, Philjae; Choi, Moon-Gun; Jeong, Kyu-Sung; Journal of the American Chemical Society 138 (2016) 92–95; doi:10.1021/jacs.5b11808

data_4129913
_publ_section_title
;
 Folding-Generated Molecular Tubes Containing One-Dimensional Water
 Chains.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              92
_journal_page_last               95
_journal_paper_doi               10.1021/jacs.5b11808
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C141 H128.2 N11 O2.6, 2.4(H2 O)'
_chemical_formula_sum            'C141 H133 N11 O5'
_chemical_formula_weight         2061.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.79(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.337(5)
_cell_length_b                   10.843(2)
_cell_length_c                   42.890(9)
_cell_measurement_reflns_used    198266
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.868
_cell_measurement_theta_min      2.290
_cell_volume                     11293(4)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            80089
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.290
_diffrn_source                   'Fixed gap multiple wiggler beamline'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   Multi-scans
_exptl_absorpt_process_details   HKL3000
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1832
_refine_ls_number_reflns         24338
_refine_ls_number_restraints     299
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1489P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2122
_refine_ls_wR_factor_ref         0.2463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13246
_reflns_number_total             24338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b11808_si_001.cif
_cod_data_source_block           Heptamer_6
_cod_database_code               4129913
_olex2_refinement_description
;
1. Others
 Fixed Sof: O116(0.6) H116(0.6) C113(0.6) C114(0.6) C115(0.6) C117(0.6)
 H11A(0.6) H11B(0.6) H11C(0.6) C118(0.6) H11D(0.6) H11E(0.6) H11F(0.6)
 O216(0.3) H216(0.3) C213(0.3) C214(0.3) C215(0.3) C217(0.3) H21A(0.3)
 H21B(0.3) H21C(0.3) C218(0.3) H21D(0.3) H21E(0.3) H21F(0.3) O316(0.1)
 H316(0.1) C313(0.1) C314(0.1) C315(0.1) C317(0.1) H31A(0.1) H31B(0.1)
 H31C(0.1) C318(0.1) H31D(0.1) H31E(0.1) H31F(0.1) O157(0.675) H15M(0.675)
 H15N(0.675) O158(0.325) H15Q(0.325) H15R(0.325) O159(0.4) H15S(0.4) H15T(0.4)
 O155(0.6) H15U(0.6) H15V(0.6)
 Fixed Uiso: H3(0.061) H6(0.066) H23(0.095) H26(0.074) H43(0.058) H46(0.082)
 H63(0.079) H66(0.075) H9(0.074) H11(0.077) H14(0.078) H15(0.08) H18(0.07)
 H20(0.062) H29(0.056) H31(0.06) H34(0.096) H35(0.103) H38(0.084) H40(0.075)
 H49(0.094) H51(0.072) H54(0.069) H55(0.07) H58(0.068) H60(0.066) H69(0.082)
 H71(0.078) H74(0.08) H75(0.078) H78(0.088) H80(0.091) H84(0.073) H85(0.081)
 H86(0.078) H90(0.066) H91(0.073) H92(0.068) H96(0.06) H97(0.062) H98(0.066)
 H12A(0.166) H12B(0.166) H12C(0.166) H12D(0.154) H12E(0.154) H12F(0.154)
 H12G(0.147) H12H(0.147) H12I(0.147) H13A(0.135) H13B(0.135) H13C(0.135)
 H13D(0.146) H13E(0.146) H13F(0.146) H13G(0.141) H13H(0.141) H13I(0.141)
 H14A(0.137) H14B(0.137) H14C(0.137) H14D(0.15) H14E(0.15) H14F(0.15)
 H14G(0.112) H14H(0.112) H14I(0.112) H15A(0.103) H15B(0.103) H15C(0.103)
 H15D(0.099) H15E(0.099) H15F(0.099) H15G(0.111) H15H(0.111) H15I(0.111)
 H116(0.078) H120(0.078) H11A(0.099) H11B(0.099) H11C(0.099) H11D(0.108)
 H11E(0.108) H11F(0.108) H12J(0.081) H12K(0.081) H12L(0.081) H12M(0.081)
 H12N(0.081) H12O(0.081) H12P(0.147) H12Q(0.147) H12R(0.147) H12S(0.193)
 H12T(0.193) H12U(0.193) H13J(0.157) H13K(0.157) H13L(0.157) H13M(0.193)
 H13N(0.193) H13O(0.193) H13P(0.194) H13Q(0.194) H13R(0.194) H13S(0.24)
 H13T(0.24) H13U(0.24) H14J(0.095) H14K(0.095) H14L(0.095) H14M(0.087)
 H14N(0.087) H14O(0.087) H14P(0.096) H14Q(0.096) H14R(0.096) H14S(0.173)
 H14T(0.173) H14U(0.173) H14V(0.12) H14W(0.12) H14X(0.12) H15J(0.137)
 H15K(0.137) H15L(0.137) H216(0.095) H220(0.061) H21A(0.099) H21B(0.099)
 H21C(0.099) H21D(0.095) H21E(0.095) H21F(0.095) H22A(0.07) H22B(0.07)
 H22C(0.07) H22D(0.066) H22E(0.066) H22F(0.066) H22G(0.145) H22H(0.145)
 H22I(0.145) H22J(0.131) H22K(0.131) H22L(0.131) H23A(0.145) H23B(0.145)
 H23C(0.145) H23D(0.105) H23E(0.105) H23F(0.105) H23G(0.128) H23H(0.128)
 H23I(0.128) H23J(0.098) H23K(0.098) H23L(0.098) H24A(0.123) H24B(0.123)
 H24C(0.123) H24D(0.162) H24E(0.162) H24F(0.162) H24G(0.117) H24H(0.117)
 H24I(0.117) H24J(0.13) H24K(0.13) H24L(0.13) H24M(0.128) H24N(0.128)
 H24O(0.128) H25A(0.143) H25B(0.143) H25C(0.143) H316(0.059) H320(0.093)
 H31A(0.073) H31B(0.073) H31C(0.073) H31D(0.066) H31E(0.066) H31F(0.066)
 H32A(0.079) H32B(0.079) H32C(0.079) H32D(0.098) H32E(0.098) H32F(0.098)
 H15M(0.106) H15N(0.106) H15O(0.12) H15P(0.12) H15Q(0.143) H15R(0.143)
 H15S(0.121) H15T(0.121) H15U(0.085) H15V(0.085)
 Fixed X: H3(0.856) H6(0.7439) H23(0.794) H26(0.847) H43(0.6635) H46(0.7453)
 H63(0.7257) H66(0.6679) H9(0.5603) H11(0.6464) H14(0.7546) H15(0.8484)
 H18(0.9572) H20(1.0444) H29(0.9763) H31(1.0587) H34(1.0319) H35(0.9885)
 H38(0.9119) H40(0.7459) H49(0.8617) H51(0.7018) H54(0.5955) H55(0.526)
 H58(0.461) H60(0.4942) H69(0.5325) H71(0.4587) H74(0.4929) H75(0.5425)
 H78(0.6269) H80(0.789) H84(0.57) H85(0.502) H86(0.526) H90(0.8157) H91(0.7368)
 H92(0.6595) H96(0.9494) H97(1.0094) H98(0.9741) H12A(0.436) H12B(0.3737)
 H12C(0.4121) H12D(0.4463) H12E(0.3947) H12F(0.456) H12G(0.3815) H12H(0.3526)
 H12I(0.4002) H13A(0.379) H13B(0.3317) H13C(0.3784) H13D(0.415) H13E(0.3535)
 H13F(0.4007) H13G(0.3977) H13H(0.3533) H13I(0.4157) H14A(0.7998) H14B(0.8407)
 H14C(0.865) H14D(0.7885) H14E(0.7973) H14F(0.7548) H14G(0.9221) H14H(0.8952)
 H14I(0.8948) H15A(1.0369) H15B(1.1016) H15C(1.0766) H15D(1.0485) H15E(1.0833)
 H15F(1.0181) H15G(1.1189) H15H(1.1443) H15I(1.1082) H116(0.7496) H120(0.9486)
 H11A(0.7854) H11B(0.7406) H11C(0.7221) H11D(0.7722) H11E(0.7823) H11F(0.8165)
 H12J(0.8909) H12K(0.9265) H12L(0.9281) H12M(1.0329) H12N(1.0295) H12O(1.0591)
 H12P(0.6334) H12Q(0.6552) H12R(0.6306) H12S(0.7996) H12T(0.7571) H12U(0.7651)
 H13J(0.706) H13K(0.7382) H13L(0.7678) H13M(0.8677) H13N(0.8625) H13O(0.8754)
 H13P(0.726) H13Q(0.7718) H13R(0.7571) H13S(0.8156) H13T(0.8025) H13U(0.7535)
 H14J(1.0933) H14K(1.1488) H14L(1.1188) H14M(1.0567) H14N(1.1134) H14O(1.0561)
 H14P(1.1228) H14Q(1.1469) H14R(1.0906) H14S(0.4909) H14T(0.4665) H14U(0.4979)
 H14V(0.575) H14W(0.5136) H14X(0.5646) H15J(0.5684) H15K(0.5331) H15L(0.5974)
 H216(0.7739) H220(0.9327) H21A(0.771) H21B(0.7764) H21C(0.8131) H21D(0.7606)
 H21E(0.7129) H21F(0.698) H22A(1.0536) H22B(1.0302) H22C(1.0356) H22D(0.8978)
 H22E(0.95) H22F(0.9258) H22G(0.6656) H22H(0.6592) H22I(0.6235) H22J(0.7795)
 H22K(0.7425) H22L(0.7475) H23A(0.6634) H23B(0.6895) H23C(0.7284) H23D(0.8099)
 H23E(0.8479) H23F(0.8669) H23G(0.7388) H23H(0.7738) H23I(0.7319) H23J(0.8766)
 H23K(0.8575) H23L(0.8273) H24A(1.0488) H24B(1.0964) H24C(1.0375) H24D(1.1252)
 H24E(1.1671) H24F(1.1369) H24G(1.0555) H24H(1.1204) H24I(1.0969) H24J(0.5351)
 H24K(0.5043) H24L(0.5697) H24M(0.4936) H24N(0.4605) H24O(0.4877) H25A(0.581)
 H25B(0.5156) H25C(0.5417) H316(0.792) H320(0.8964) H31A(0.8278) H31B(0.7743)
 H31C(0.776) H31D(0.7746) H31E(0.7546) H31F(0.8172) H32A(1.0445) H32B(1.0079)
 H32C(1.0177) H32D(0.9196) H32E(0.9456) H32F(0.9846) H15M(0.7896) H15N(0.7337)
 H15O(0.7454) H15P(0.7807) H15Q(0.7834) H15R(0.8303) H15S(0.7427) H15T(0.7375)
 H15U(0.7661) H15V(0.7676)
 Fixed Y: H3(1.0175) H6(0.9483) H23(0.6802) H26(0.7063) H43(0.4929)
 H46(0.4424) H63(0.2919) H66(0.1796) H9(0.8495) H11(1.0101) H14(1.089)
 H15(1.1269) H18(1.1569) H20(1.139) H29(0.7619) H31(0.715) H34(0.6739)
 H35(0.6587) H38(0.6699) H40(0.6855) H49(0.3181) H51(0.2884) H54(0.3112)
 H55(0.3385) H58(0.4177) H60(0.5529) H69(0.0138) H71(0.1126) H74(0.2197)
 H75(0.2972) H78(0.3772) H80(0.4538) H84(0.6277) H85(0.6503) H86(0.7287)
 H90(0.7961) H91(0.7687) H92(0.6722) H96(0.4182) H97(0.4268) H98(0.4131) H12A(-
 0.1663) H12B(-0.1184) H12C(-0.0832) H12D(0.0602) H12E(-0.0301) H12F(-0.0823)
 H12G(0.1296) H12H(0.0943) H12I(0.1963) H13A(0.5464) H13B(0.4849) H13C(0.4004)
 H13D(0.6334) H13E(0.6243) H13F(0.6874) H13G(0.3123) H13H(0.4001) H13I(0.3995)
 H14A(0.8744) H14B(0.8534) H14C(0.8799) H14D(0.5497) H14E(0.6436) H14F(0.6764)
 H14G(0.6943) H14H(0.661) H14I(0.5617) H15A(1.1105) H15B(1.138) H15C(1.0247)
 H15D(1.3826) H15E(1.3515) H15F(1.3296) H15G(1.1079) H15H(1.2178) H15I(1.2481)
 H116(-0.1558) H120(1.2685) H11A(-0.0278) H11B(0.0803) H11C(-0.0603)
 H11D(0.0395) H11E(0.1346) H11F(0.0086) H12J(1.0806) H12K(0.9599) H12L(1.075)
 H12M(1.0704) H12N(0.9626) H12O(1.0902) H12P(0.5081) H12Q(0.4384) H12R(0.3609)
 H12S(0.4835) H12T(0.5503) H12U(0.6) H13J(0.2399) H13K(0.3217) H13L(0.284)
 H13M(0.3356) H13N(0.312) H13O(0.1994) H13P(0.2601) H13Q(0.283) H13R(0.39)
 H13S(0.0685) H13T(0.0485) H13U(0.078) H14J(0.5831) H14K(0.6621) H14L(0.6138)
 H14M(0.8926) H14N(0.8259) H14O(0.7557) H14P(0.8371) H14Q(0.8825) H14R(0.9393)
 H14S(0.961) H14T(0.883) H14U(0.8143) H14V(0.9309) H14W(0.9823) H14X(1.0583)
 H15J(0.7121) H15K(0.7645) H15L(0.7952) H216(-0.135) H220(0.8964) H21A(0.1519)
 H21B(0.1615) H21C(0.0643) H21D(-0.0545) H21E(0.0464) H21F(-0.0912)
 H22A(1.0705) H22B(0.9671) H22C(0.9387) H22D(1.129) H22E(1.215) H22F(1.2045)
 H22G(0.6421) H22H(0.601) H22I(0.5345) H22J(0.5002) H22K(0.5788) H22L(0.6199)
 H23A(0.3215) H23B(0.3962) H23C(0.317) H23D(0.4277) H23E(0.3292) H23F(0.3847)
 H23G(0.136) H23H(0.1822) H23I(0.2743) H23J(0.1707) H23K(0.1187) H23L(0.0732)
 H24A(0.8951) H24B(0.8246) H24C(0.7607) H24D(0.6842) H24E(0.7295) H24F(0.8283)
 H24G(0.5721) H24H(0.5885) H24I(0.5435) H24J(0.7296) H24K(0.752) H24L(0.7351)
 H24M(1.0395) H24N(0.931) H24O(0.9077) H25A(1.0094) H25B(0.993) H25C(1.0878)
 H316(-0.1327) H320(0.9749) H31A(0.1287) H31B(0.1503) H31C(0.2014) H31D(0.0517)
 H31E(-0.0871) H31F(-0.0493) H32A(1.0413) H32B(1) H32C(0.9064) H32D(1.2113)
 H32E(1.1439) H32F(1.2168) H15M(0.2744) H15N(0.2729) H15O(0.5685) H15P(0.4857)
 H15Q(0.9585) H15R(1.0007) H15S(0.6214) H15T(0.7229) H15U(0.7207) H15V(0.8444)
 Fixed Z: H3(0.6365) H6(0.6375) H23(0.5376) H26(0.5974) H43(0.6135)
 H46(0.5757) H63(0.6659) H66(0.6152) H9(0.6675) H11(0.7398) H14(0.7532)
 H15(0.7538) H18(0.7393) H20(0.6625) H29(0.6865) H31(0.6088) H34(0.5448)
 H35(0.4954) H38(0.4423) H40(0.4269) H49(0.4954) H51(0.4632) H54(0.4908)
 H55(0.5247) H58(0.576) H60(0.6629) H69(0.5395) H71(0.6173) H74(0.6767)
 H75(0.7203) H78(0.7659) H80(0.7664) H84(0.4915) H85(0.5277) H86(0.577)
 H90(0.7326) H91(0.761) H92(0.7369) H96(0.6931) H97(0.6529) H98(0.6011)
 H12A(0.5728) H12B(0.5692) H12C(0.5996) H12D(0.5148) H12E(0.517) H12F(0.5231)
 H12G(0.5866) H12H(0.5532) H12I(0.5558) H13A(0.5805) H13B(0.5995) H13C(0.5859)
 H13D(0.6589) H13E(0.6434) H13F(0.6246) H13G(0.6383) H13H(0.653) H13I(0.6673)
 H14A(0.3922) H14B(0.3649) H14C(0.3998) H14D(0.38) H14E(0.3519) H14F(0.3776)
 H14G(0.3961) H14H(0.3621) H14I(0.3897) H15A(0.7647) H15B(0.766) H15C(0.7458)
 H15D(0.7178) H15E(0.7498) H15F(0.7469) H15G(0.6988) H15H(0.7201) H15I(0.6884)
 H116(0.5734) H120(0.5573) H11A(0.5086) H11B(0.5049) H11C(0.4999) H11D(0.5888)
 H11E(0.5612) H11F(0.564) H12J(0.5458) H12K(0.5396) H12L(0.5164) H12M(0.5263)
 H12N(0.5516) H12O(0.5612) H12P(0.8088) H12Q(0.8401) H12R(0.8107) H12S(0.82)
 H12T(0.8413) H12U(0.8068) H13J(0.8173) H13K(0.8437) H13L(0.8128) H13M(0.4537)
 H13N(0.4168) H13O(0.4402) H13P(0.4201) H13Q(0.3957) H13R(0.4194) H13S(0.4632)
 H13T(0.4265) H13U(0.4486) H14J(0.6817) H14K(0.6812) H14L(0.6492) H14M(0.6994)
 H14N(0.7104) H14O(0.7133) H14P(0.6312) H14Q(0.6649) H14R(0.6497) H14S(0.6947)
 H14T(0.7223) H14U(0.6956) H14V(0.7721) H14W(0.7656) H14X(0.7538) H15J(0.7335)
 H15K(0.7607) H15L(0.7606) H216(0.5402) H220(0.5534) H21A(0.5538) H21B(0.5169)
 H21C(0.5371) H21D(0.4885) H21E(0.4832) H21F(0.4932) H22A(0.5554) H22B(0.5314)
 H22C(0.5681) H22D(0.5373) H22E(0.5325) H22F(0.5662) H22G(0.7956) H22H(0.831)
 H22I(0.8032) H22J(0.8146) H22K(0.8368) H22L(0.8012) H23A(0.8192) H23B(0.8487)
 H23C(0.8277) H23D(0.4241) H23E(0.4079) H23F(0.4415) H23G(0.4294) H23H(0.4013)
 H23I(0.4167) H23J(0.4624) H23K(0.4285) H23L(0.4584) H24A(0.6996) H24B(0.72)
 H24C(0.7132) H24D(0.6378) H24E(0.6658) H24F(0.6429) H24G(0.6969) H24H(0.7041)
 H24I(0.6703) H24J(0.7101) H24K(0.7414) H24L(0.7431) H24M(0.7059) H24N(0.7216)
 H24O(0.6891) H25A(0.7656) H25B(0.7652) H25C(0.7417) H316(0.5862) H320(0.541)
 H31A(0.5868) H31B(0.6058) H31C(0.5709) H31D(0.5253) H31E(0.5304) H31F(0.5395)
 H32A(0.5568) H32B(0.5262) H32C(0.5549) H32D(0.5504) H32E(0.5216) H32F(0.5468)
 H15M(0.628) H15N(0.6193) H15O(0.6408) H15P(0.6277) H15Q(0.5963) H15R(0.583)
 H15S(0.5892) H15T(0.5682) H15U(0.6055) H15V(0.5973)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'