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_4129912
_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         'C176 H156 N14 O2, 0.85(C5 H12), 5(H2 O)'
_chemical_formula_sum            'C180.24 H176.19 N14 O7'
_chemical_formula_weight         2650.47
_chemical_name_common            nonamer1
_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     iterative
_audit_creation_date             2015-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                71.612(4)
_cell_angle_beta                 71.701(4)
_cell_angle_gamma                75.717(4)
_cell_formula_units_Z            2
_cell_length_a                   18.3781(16)
_cell_length_b                   20.5298(19)
_cell_length_c                   25.009(2)
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.25
_cell_volume                     8386.3(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1497
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            315860
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.128
_diffrn_reflns_theta_min         2.252
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0867 before and 0.0757 after correction.
The Ratio of minimum to maximum transmission is 0.9325.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       block
_exptl_crystal_F_000             2823
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1881
_refine_ls_number_reflns         33282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0625
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19883
_reflns_number_total             33282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b11808_si_002.cif
_cod_data_source_block           Nonamer_7
_cod_database_code               4129912
_olex2_refinement_description
;The voids contain disordered solvent at partial occupancy. A
satisfactory disorder model for the solvent was not found, and therefore the
OLEX2 Solvent Mask routine (similar to PLATON/SQUEEZE) was used to mask out the
disordered density.

1. Others
 Fixed Uiso: H148(0.05) H3(0.031) H6(0.03) H23(0.027) H26(0.03) H43(0.03)
 H46(0.029) H63(0.028) H66(0.028) H83(0.029) H86(0.032) H9(0.036) H11(0.033)
 H14(0.034) H15(0.036) H18(0.036) H20(0.035) H29(0.038) H31(0.035) H34(0.032)
 H35(0.031) H38(0.031) H40(0.032) H49(0.033) H51(0.036) H54(0.04) H55(0.04)
 H58(0.038) H60(0.037) H69(0.033) H71(0.034) H74(0.037) H75(0.035) H78(0.035)
 H80(0.036) H89(0.042) H91(0.04) H94(0.04) H95(0.039) H98(0.035) H100(0.032)
 H104(0.036) H105(0.037) H106(0.035) H110(0.037) H111(0.04) H112(0.038)
 H116(0.037) H117(0.042) H118(0.036) H122(0.03) H123(0.032) H124(0.031)
 H14A(0.07) H14B(0.07) H14C(0.07) H14D(0.067) H14E(0.067) H14F(0.067)
 H15A(0.063) H15B(0.063) H15C(0.063) H15D(0.069) H15E(0.069) H15F(0.069)
 H15G(0.073) H15H(0.073) H15I(0.073) H15J(0.071) H15K(0.071) H15L(0.071)
 H15M(0.066) H15N(0.066) H15O(0.066) H15P(0.072) H15Q(0.072) H15R(0.072)
 H15S(0.061) H15T(0.061) H15U(0.061) H16A(0.079) H16B(0.079) H16C(0.079)
 H16D(0.061) H16E(0.061) H16F(0.061) H16G(0.064) H16H(0.064) H16I(0.064)
 H16J(0.059) H16K(0.059) H16L(0.059) H16M(0.098) H16N(0.098) H16O(0.098)
 H16P(0.08) H16Q(0.08) H16R(0.08) H16S(0.087) H16T(0.087) H16U(0.087)
 H17A(0.086) H17B(0.086) H17C(0.086) H17D(0.111) H17E(0.111) H17F(0.111)
 H17G(0.145) H17H(0.145) H17I(0.145) H17J(0.077) H17K(0.077) H17L(0.077)
 H17M(0.081) H17N(0.081) H17O(0.081) H17P(0.07) H17Q(0.07) H17R(0.07) H17S(0.1)
 H17T(0.1) H17U(0.1) H17V(0.087) H17W(0.087) H17X(0.087) H18A(0.08) H18B(0.08)
 H18C(0.08) H18D(0.07) H18E(0.07) H18F(0.07) H18G(0.069) H18H(0.069)
 H18I(0.069) H18J(0.065) H18K(0.065) H18L(0.065) H18M(0.06) H18N(0.06)
 H18O(0.06) H18P(0.074) H18Q(0.074) H18R(0.074) H18S(0.077) H18T(0.077)
 H18U(0.077) H19A(0.096) H19B(0.096) H19C(0.096) H19D(0.079) H19E(0.079)
 H19F(0.079) H19G(0.109) H19H(0.109) H19I(0.109) H30A(0.167) H30B(0.167)
 H30C(0.167) H30D(0.111) H30E(0.111) H30F(0.153) H30G(0.153) H30H(0.163)
 H30I(0.163) H30J(0.213) H30K(0.213) H30L(0.213) H20A(0.064) H20B(0.064)
 H20C(0.046) H20D(0.046) H20E(0.051) H20F(0.051) H20G(0.047) H20H(0.047)
 Fixed X: H148(0.851) H3(0.6391) H6(0.5211) H23(0.7232) H26(0.679) H43(0.4659)
 H46(0.6039) H63(0.4744) H66(0.3948) H83(0.4987) H86(0.3509) H9(0.2893)
 H11(0.2543) H14(0.3376) H15(0.4317) H18(0.5704) H20(0.793) H29(0.6739)
 H31(0.8867) H34(0.9594) H35(0.9931) H38(1.0024) H40(0.8588) H49(0.8335)
 H51(0.7337) H54(0.5973) H55(0.4799) H58(0.3412) H60(0.2374) H69(0.2164)
 H71(0.1176) H74(0.1602) H75(0.2257) H78(0.34) H80(0.5632) H89(0.1222)
 H91(0.2963) H94(0.4541) H95(0.573) H98(0.6999) H100(0.7491) H104(0.5893)
 H105(0.4705) H106(0.4127) H110(0.2601) H111(0.2967) H112(0.4217) H116(0.7798)
 H117(0.8815) H118(0.8631) H122(0.6506) H123(0.5928) H124(0.4775) H14A(0.9414)
 H14B(0.9825) H14C(0.9881) H14D(0.933) H14E(0.9222) H14F(0.8491) H15A(0.1456)
 H15B(0.1129) H15C(0.2044) H15D(0.0959) H15E(0.0446) H15F(0.0792) H15G(0.6975)
 H15H(0.7499) H15I(0.7851) H15J(0.8218) H15K(0.7887) H15L(0.7592) H15M(0.6231)
 H15N(0.6613) H15O(0.6009) H15P(0.1264) H15Q(0.0802) H15R(0.1601) H15S(0.2159)
 H15T(0.132) H15U(0.208) H16A(0.1583) H16B(0.079) H16C(0.1262) H16D(0.9767)
 H16E(1.0641) H16F(1.043) H16G(0.9727) H16H(1.0247) H16I(0.9357) H16J(1.1007)
 H16K(1.1204) H16L(1.0699) H16M(0.802) H16N(0.8645) H16O(0.8863) H16P(0.9228)
 H16Q(0.8985) H16R(0.8605) H16S(0.7285) H16T(0.7731) H16U(0.7101) H17A(0.1238)
 H17B(0.1092) H17C(0.1591) H17D(0.266) H17E(0.2222) H17F(0.3068) H17G(0.2431)
 H17H(0.1596) H17I(0.1732) H17J(0.8095) H17K(0.9023) H17L(0.8616) H17M(0.8457)
 H17N(0.8868) H17O(0.795) H17P(0.9457) H17Q(0.9792) H17R(0.9411) H17S(0.4317)
 H17T(0.4783) H17U(0.5227) H17V(0.3682) H17W(0.3833) H17X(0.3367) H18A(0.5697)
 H18B(0.5204) H18C(0.5089) H18D(0.0638) H18E(0.0278) H18F(0.1193) H18G(0.0204)
 H18H(-0.0334) H18I(0.0078) H18J(0.1362) H18K(0.0436) H18L(0.0936) H18M(0.8231)
 H18N(0.9024) H18O(0.8708) H18P(0.7649) H18Q(0.836) H18R(0.7522) H18S(0.8743)
 H18T(0.9114) H18U(0.8361) H19A(0.1957) H19B(0.1462) H19C(0.2303) H19D(0.0456)
 H19E(0.0381) H19F(0.087) H19G(0.1718) H19H(0.0883) H19I(0.1003) H30A(0.7473)
 H30B(0.7239) H30C(0.8099) H30D(0.7574) H30E(0.6725) H30F(0.7104) H30G(0.7958)
 H30H(0.6642) H30I(0.7507) H30J(0.785) H30K(0.6939) H30L(0.729) H20A(0.6538)
 H20B(0.7228) H20C(0.5941) H20D(0.6112) H20E(0.5421) H20F(0.5015) H20G(0.5262)
 H20H(0.5879)
 Fixed Y: H148(0.5599) H3(0.6872) H6(0.6066) H23(0.4138) H26(0.5547)
 H43(0.4396) H46(0.4143) H63(0.6908) H66(0.5848) H83(0.6418) H86(0.7137)
 H9(0.5239) H11(0.734) H14(0.8385) H15(0.9049) H18(0.9543) H20(0.8707)
 H29(0.8009) H31(0.6961) H34(0.5541) H35(0.4344) H38(0.2929) H40(0.1825)
 H49(0.3146) H51(0.1614) H54(0.1518) H55(0.1728) H58(0.2324) H60(0.4266)
 H69(0.4322) H71(0.6314) H74(0.7694) H75(0.8601) H78(0.9454) H80(0.9092)
 H89(0.8831) H91(0.9795) H94(0.9351) H95(0.8719) H98(0.7636) H100(0.5547)
 H104(0.1911) H105(0.2115) H106(0.3261) H110(0.6825) H111(0.792) H112(0.799)
 H116(0.7257) H117(0.6321) H118(0.521) H122(0.3506) H123(0.2664) H124(0.3009)
 H14A(0.6353) H14B(0.6542) H14C(0.5747) H14D(0.5475) H14E(0.6271) H14F(0.587)
 H15A(0.5569) H15B(0.637) H15C(0.6094) H15D(0.6208) H15E(0.6445) H15F(0.564)
 H15G(1.0075) H15H(1.0593) H15I(0.9788) H15J(0.9651) H15K(1.0449) H15L(0.9845)
 H15M(1.0432) H15N(1.0984) H15O(1.056) H15P(0.7274) H15Q(0.6968) H15R(0.724)
 H15S(0.6091) H15T(0.5882) H15U(0.5391) H16A(0.5438) H16B(0.5891) H16C(0.6171)
 H16D(0.1534) H16E(0.1181) H16F(0.2007) H16G(0.1035) H16H(0.0601) H16I(0.0911)
 H16J(0.2167) H16K(0.1348) H16L(0.1848) H16M(0.8263) H16N(0.8729) H16O(0.7898)
 H16P(0.7954) H16Q(0.8782) H16R(0.8321) H16S(0.8902) H16T(0.934) H16U(0.8902)
 H17A(0.3624) H17B(0.3215) H17C(0.3835) H17D(0.3116) H17E(0.2456) H17F(0.2397)
 H17G(0.1958) H17H(0.2115) H17I(0.2458) H17J(0.0881) H17K(0.0721) H17L(0.1023)
 H17M(0.2263) H17N(0.1469) H17O(0.1652) H17P(0.1973) H17Q(0.1622) H17R(0.2427)
 H17S(1.0292) H17T(1.087) H17U(1.0097) H17V(1.0516) H17W(1.1113) H17X(1.0515)
 H18A(1.0079) H18B(1.083) H18C(1.0178) H18D(0.5806) H18E(0.5127) H18F(0.512)
 H18G(0.5183) H18H(0.5206) H18I(0.5858) H18J(0.4037) H18K(0.4119) H18L(0.4078)
 H18M(0.5585) H18N(0.5897) H18O(0.5655) H18P(0.7412) H18Q(0.6901) H18R(0.667)
 H18S(0.6834) H18T(0.702) H18U(0.7511) H19A(1.0661) H19B(1.1161) H19C(1.075)
 H19D(0.9728) H19E(1.0546) H19F(1.0002) H19G(1.0255) H19H(1.0668) H19I(0.9844)
 H30A(0.1409) H30B(0.0697) H30C(0.071) H30D(0.0973) H30E(0.0929) H30F(-0.0231)
 H30G(-0.0191) H30H(-0.002) H30I(-0.0002) H30J(-0.1226) H30K(-0.1223) H30L(-
 0.114) H20A(0.5467) H20B(0.5765) H20C(0.4843) H20D(0.4345) H20E(0.535)
 H20F(0.5528) H20G(0.5479) H20H(0.5855)
 Fixed Z: H148(0.5674) H3(0.5104) H6(0.5377) H23(0.6713) H26(0.6671)
 H43(0.7449) H46(0.7789) H63(0.7986) H66(0.825) H83(0.924) H86(0.9231)
 H9(0.5522) H11(0.5037) H14(0.4839) H15(0.4674) H18(0.4456) H20(0.4474)
 H29(0.6306) H31(0.6462) H34(0.6707) H35(0.6826) H38(0.6801) H40(0.6653)
 H49(0.8506) H51(0.8492) H54(0.8248) H55(0.8009) H58(0.7632) H60(0.6964)
 H69(0.8584) H71(0.8003) H74(0.7762) H75(0.7588) H78(0.7419) H80(0.7486)
 H89(0.9044) H91(0.8908) H94(0.903) H95(0.9171) H98(0.942) H100(0.9662)
 H104(0.6604) H105(0.6365) H106(0.6023) H110(0.6577) H111(0.6326) H112(0.632)
 H116(0.7964) H117(0.8066) H118(0.8131) H122(0.9605) H123(0.9514) H124(0.9212)
 H14A(0.5389) H14B(0.4705) H14C(0.5077) H14D(0.4386) H14E(0.4018) H14F(0.43)
 H15A(1.0661) H15B(1.0648) H15C(1.0527) H15D(0.9292) H15E(0.9867) H15F(0.9905)
 H15G(0.5) H15H(0.4491) H15I(0.4697) H15J(0.3714) H15K(0.3455) H15L(0.3342)
 H15M(0.375) H15N(0.3858) H15O(0.4385) H15P(0.5332) H15Q(0.5044) H15R(0.4666)
 H15S(0.4428) H15T(0.4773) H15U(0.4943) H16A(0.5978) H16B(0.5836) H16C(0.6135)
 H16D(0.5953) H16E(0.5972) H16F(0.5739) H16G(0.7477) H16H(0.7019) H16I(0.7024)
 H16J(0.6433) H16K(0.6711) H16L(0.712) H16M(0.7065) H16N(0.6612) H16O(0.6772)
 H16P(0.5706) H16Q(0.5547) H16R(0.5332) H16S(0.5814) H16T(0.5999) H16U(0.6483)
 H17A(0.7446) H17B(0.705) H17C(0.6754) H17D(0.6273) H17E(0.6543) H17F(0.6624)
 H17G(0.7704) H17H(0.7576) H17I(0.8022) H17J(0.9039) H17K(0.8908) H17L(0.838)
 H17M(0.9419) H17N(0.9574) H17O(0.9643) H17P(0.8013) H17Q(0.8575) H17R(0.8441)
 H17S(0.8073) H17T(0.7586) H17U(0.7791) H17V(0.6807) H17W(0.7025) H17X(0.7481)
 H18A(0.6748) H18B(0.6546) H18C(0.6378) H18D(0.7539) H18E(0.7646) H18F(0.7385)
 H18G(0.9091) H18H(0.869) H18I(0.857) H18J(0.8222) H18K(0.8444) H18L(0.8878)
 H18M(1.023) H18N(0.9986) H18O(0.9564) H18P(1.0118) H18Q(1.0351) H18R(1.0565)
 H18S(0.8853) H18T(0.9276) H18U(0.9092) H19A(0.9156) H19B(0.8713) H19C(0.8469)
 H19D(0.9361) H19E(0.9275) H19F(0.9704) H19G(0.7938) H19H(0.8191) H19I(0.8287)
 H30A(0.6234) H30B(0.6259) H30C(0.6275) H30D(0.721) H30E(0.7195) H30F(0.7221)
 H30G(0.7221) H30H(0.8114) H30I(0.8114) H30J(0.8025) H30K(0.8162) H30L(0.8643)
 H20A(0.563) H20B(0.5379) H20C(0.66) H20D(0.6274) H20E(0.7533) H20F(0.7094)
 H20G(0.8411) H20H(0.8072)
;
_shelx_hkl_checksum              30274
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'