Terpyridine-Based, Flexible Tripods: From a Highly Symmetric Nanosphere to Temperature-Dependent, Irreversible, 3D Isomeric Macromolecular Nanocages.
Chakraborty, Sourav; Hong, Wei; Endres, Kevin J.; Xie, Ting-Zheng; Wojtas, Lukasz; Moorefield, Charles N.; Wesdemiotis, Chrys; Newkome, George R.; Journal of the American Chemical Society 139 (2017) 3012–3020; doi:10.1021/jacs.6b11784

data_4125482
_publ_section_title
;
 Terpyridine-Based, Flexible Tripods: From a Highly Symmetric Nanosphere
 to Temperature-Dependent, Irreversible, 3D Isomeric Macromolecular
 Nanocages.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3012
_journal_page_last               3020
_journal_paper_doi               10.1021/jacs.6b11784
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C324 H216 N40 Ru6'
_chemical_formula_sum            'C324 H216 N40 Ru6'
_chemical_formula_weight         5275.78
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   30.4451(13)
_cell_length_b                   30.4451(13)
_cell_length_c                   96.083(4)
_cell_measurement_reflns_used    5908
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      49.46
_cell_measurement_theta_min      2.49
_cell_volume                     77128(6)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            11875
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.949
_diffrn_reflns_theta_max         26.949
_diffrn_reflns_theta_min         3.384
_diffrn_source                   'INCOATEC Imus micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  0.7499
_exptl_absorpt_correction_T_min  0.5314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1479 before and 0.0632 after correction.
The Ratio of minimum to maximum transmission is 0.7086.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.682
_exptl_crystal_description       block
_exptl_crystal_F_000             16224
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
Structural voids presumably 
contain a mixture of DMF and ethyl acetate
;
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     571
_refine_ls_restrained_S_all      1.772
_refine_ls_R_factor_all          0.1896
_refine_ls_R_factor_gt           0.1360
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4004
_refine_ls_wR_factor_ref         0.4491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2214
_reflns_number_total             3580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11784_si_002.cif
_cod_data_source_block           xie_sc_ne_1_res1_5_sq
_cod_depositor_comments          'Adding full bibliography for 4125482.cif.'
_cod_original_cell_volume        77128(7)
_cod_database_code               4125482
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-C62 = N1-C92 = N1-C2 = N1-C32 = N131-C172 = N131-C132
 1.43 with sigma of 0.02
 Ru1_$1-N115 = Ru1_$1-N121
 2.07 with sigma of 0.02
 Ru1_$1-N107
 1.97 with sigma of 0.02
 Ru1-N77 = Ru2-N187 = Ru3-N147 = Ru3-N47 = Ru2-N17
 1.97 with sigma of 0.02
 Ru1-N85 = Ru1-N91 = Ru3-N155 = Ru3-N161 = Ru3-N55 = Ru3-N61 = Ru2-N25 = Ru2-
 N31 = Ru2-N201 = Ru2-N195
 2.07 with sigma of 0.02
 C110-C108 = C116-C106 = C104-C102 = C98-C95 = C80-C76 = C86-C78 = C74-C72 =
 C68-C65 = C38-C35 = C8-C5 = C44-C40 = C14-C12 = C50-C48 = C56-C46 = C26-C16 =
 C20-C18 = C190-C186 = C196-C188 = C156-C146 = C150-C148 = C182-C184 = C144-
 C142 = C178-C175 = C138-C135
 1.48 with sigma of 0.02
 C104-C103 = C109-C102
 2.51 with sigma of 0.04
 C104-C101 = C102-C105
 2.51 with sigma of 0.04
 C98-C94 = C95-C99
 2.51 with sigma of 0.04
 C98-C96 = C95-C103
 2.51 with sigma of 0.04
 C65-C73 = C68-C66
 2.51 with sigma of 0.04
 C65-C69 = C68-C64
 2.51 with sigma of 0.04
 C35-C43 = C38-C36
 2.51 with sigma of 0.04
 C38-C34 = C35-C39
 2.51 with sigma of 0.04
 C5-C13 = C8-C6
 2.51 with sigma of 0.04
 C5-C9 = C8-C4
 2.51 with sigma of 0.04
 C40-C49 = C44-C41
 2.51 with sigma of 0.04
 C40-C45 = C44-C39
 2.51 with sigma of 0.04
 C12-C19 = C14-C13
 2.51 with sigma of 0.04
 C12-C15 = C14-C11
 2.51 with sigma of 0.04
 C182-C189 = C184-C181
 2.51 with sigma of 0.04
 C184-C183 = C182-C185
 2.51 with sigma of 0.04
 C142-C145 = C144-C141
 2.51 with sigma of 0.04
 C142-C149 = C144-C143
 2.51 with sigma of 0.04
 C178-C176 = C175-C179
 2.51 with sigma of 0.04
 C138-C134 = C135-C139
 2.51 with sigma of 0.04
 C178-C174 = C175-C183
 2.51 with sigma of 0.04
 C138-C136 = C135-C143
 2.51 with sigma of 0.04
 N131-C133
 2.44 with sigma of 0.04
 N131-C177
 2.44 with sigma of 0.04
 N131-C137
 2.44 with sigma of 0.04
 N131-C173
 2.44 with sigma of 0.04
 N1-C63
 2.44 with sigma of 0.04
 N1-C67
 2.44 with sigma of 0.04
 N1-C93
 2.44 with sigma of 0.04
 N1-C97
 2.44 with sigma of 0.04
 N1-C3
 2.44 with sigma of 0.04
 N1-C7
 2.44 with sigma of 0.04
 N1-C33
 2.44 with sigma of 0.04
 N1-C37
 2.44 with sigma of 0.04
 C72-C75 = C74-C71
 2.51 with sigma of 0.04
 C72-C79 = C74-C73
 2.51 with sigma of 0.04
 N77-C80
 2.35 with sigma of 0.04
 N77-C86
 2.35 with sigma of 0.04
 N107-C116
 2.35 with sigma of 0.04
 N107-C110
 2.35 with sigma of 0.04
 N17-C20
 2.35 with sigma of 0.04
 N17-C26
 2.35 with sigma of 0.04
 N47-C50
 2.35 with sigma of 0.04
 N147-C156
 2.35 with sigma of 0.04
 N147-C150
 2.35 with sigma of 0.04
 N187-C196
 2.35 with sigma of 0.04
 N187-C190
 2.35 with sigma of 0.04
 C76-N85 = C78-N91 = C106-N121 = C108-N115 = C48-N55 = C46-N61 = C16-N31 = C18-
 N25 = C146-N161 = C148-N155 = C188-N201 = C186-N195
 2.4 with sigma of 0.04
 C106-C117 = C108-C111 = C76-C81 = C78-C87 = C18-C21 = C16-C27 = C48-C51 = C46-
 C57 = C148-C151 = C146-C157 = C188-C197 = C186-C191
 2.52 with sigma of 0.04
 N47-C56
 2.35 with sigma of 0.04
 C110-C109 = C116-C105 = C86-C79 = C80-C75 = C50-C49 = C56-C45 = C20-C19 = C26-
 C15 = C196-C189 = C190-C185 = C156-C145 = C150-C149
 2.56 with sigma of 0.04
3. Restrained planarity
 C189, C188, N187, C196
 with sigma of 0.1
 N201, C196, C197, C188
 with sigma of 0.1
 C49, C48, N47, C50
 with sigma of 0.1
 C51, C50, N55, C48
 with sigma of 0.1
 C46, C56, N61, C57
 with sigma of 0.1
 N47, C46, C45, C56
 with sigma of 0.1
 N147, C146, C145, C156
 with sigma of 0.1
 N161, C156, C157, C146
 with sigma of 0.1
 C151, C150, N155, C148
 with sigma of 0.1
 C149, C148, N147, C150
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Ru2 \\sim N1 \\sim C2 \\sim C32 \\sim C62 \\sim C92 \\sim C7 \\sim C3 \\sim C37
\\sim C33 \\sim C67 \\sim C63 \\sim C93 \\sim C97 \\sim C6 \\sim C4 \\sim C36
\\sim C34 \\sim C66 \\sim C64 \\sim C94 \\sim C96 \\sim C5 \\sim C35 \\sim C65
\\sim C95 \\sim C8 \\sim C38 \\sim C68 \\sim C98 \\sim C9 \\sim C13 \\sim C39
\\sim C43 \\sim C69 \\sim C73 \\sim C103 \\sim C99 \\sim C10 \\sim C12 \\sim
C40 \\sim C42 \\sim C70 \\sim C72 \\sim C102 \\sim C100 \\sim C11 \\sim C14
\\sim C41 \\sim C44 \\sim C71 \\sim C74 \\sim C101 \\sim C104 \\sim C19 \\sim
C15 \\sim C45 \\sim C49 \\sim C75 \\sim C79 \\sim C109 \\sim C105 \\sim C18
\\sim C16 \\sim C46 \\sim C48 \\sim C76 \\sim C78 \\sim C108 \\sim C106 \\sim
N17 \\sim C20 \\sim C26 \\sim N47 \\sim C56 \\sim C50 \\sim N77 \\sim C80 \\sim
C86 \\sim N107 \\sim C110 \\sim C116 \\sim N25 \\sim C21 \\sim N31 \\sim C27
\\sim Ru3 \\sim N61 \\sim C57 \\sim N55 \\sim C51 \\sim Ru1 \\sim C81 \\sim N85
\\sim N91 \\sim C87 \\sim C111 \\sim N115 \\sim N121 \\sim C117 \\sim N195
\\sim N201 \\sim N187 \\sim C24 \\sim C22 \\sim C30 \\sim C28 \\sim N147 \\sim
N155 \\sim N161 \\sim C60 \\sim C58 \\sim C54 \\sim C52 \\sim C82 \\sim C84
\\sim C90 \\sim C88 \\sim C112 \\sim C114 \\sim C120 \\sim C118 \\sim C190
\\sim C194 \\sim C196 \\sim C200 \\sim C188 \\sim C186 \\sim C23 \\sim C29
\\sim C148 \\sim C146 \\sim C150 \\sim C154 \\sim C156 \\sim C160 \\sim C59
\\sim C53 \\sim C83 \\sim C89 \\sim C113 \\sim C119 \\sim C191 \\sim C193 \\sim
C197 \\sim C199 \\sim C189 \\sim C185 \\sim C149 \\sim C145 \\sim C151 \\sim
C153 \\sim C157 \\sim C159 \\sim C192 \\sim C198 \\sim C184 \\sim C144 \\sim
C152 \\sim C158 \\sim C182 \\sim C142 \\sim C183 \\sim C181 \\sim C143 \\sim
C141 \\sim C178 \\sim C180 \\sim C138 \\sim C140 \\sim C175 \\sim C179 \\sim
C135 \\sim C139 \\sim C176 \\sim C174 \\sim C136 \\sim C134 \\sim C177 \\sim
C173 \\sim C137 \\sim C133 \\sim C172 \\sim C132 \\sim N131: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: C2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) C6(0.5) H6(0.5)
 C7(0.5) H7(0.5) Ru2(0.5) Ru3(0.5) C8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5)
 C11(0.5) H11(0.5) C12(0.5) C13(0.5) H13(0.5) C14(0.5) C15(0.5) H15(0.5)
 C16(0.5) N17(0.5) C18(0.5) C19(0.5) H19(0.5) C20(0.5) C21(0.5) H21(0.5)
 C22(0.5) H22(0.5) C23(0.5) H23(0.5) C24(0.5) H24(0.5) N25(0.5) C26(0.5)
 C27(0.5) H27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5) H30(0.5)
 N31(0.5) C32(0.5) C37(0.5) H37(0.5) C36(0.5) H36(0.5) C35(0.5) C34(0.5)
 H34(0.5) C33(0.5) H33(0.5) C38(0.5) C39(0.5) H39(0.5) C40(0.5) C41(0.5)
 H41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) C45(0.5) H45(0.5)
 C46(0.5) N47(0.5) C48(0.5) C49(0.5) H49(0.5) C50(0.5) C51(0.5) H51(0.5)
 C52(0.5) H52(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5) N55(0.5) C56(0.5)
 C57(0.5) H57(0.5) C58(0.5) H58(0.5) C59(0.5) H59(0.5) C60(0.5) H60(0.5)
 N61(0.5) C132(0.5) C137(0.5) H137(0.5) C136(0.5) H136(0.5) C135(0.5) C134(0.5)
 H134(0.5) C133(0.5) H133(0.5) C138(0.5) C143(0.5) H143(0.5) C142(0.5)
 C141(0.5) H141(0.5) C140(0.5) H140(0.5) C139(0.5) H139(0.5) C144(0.5)
 C149(0.5) H149(0.5) C148(0.5) N147(0.5) C146(0.5) C145(0.5) H145(0.5)
 C150(0.5) C151(0.5) H151(0.5) C152(0.5) H152(0.5) C153(0.5) H153(0.5)
 C154(0.5) H154(0.5) N155(0.5) C156(0.5) C157(0.5) H157(0.5) C158(0.5)
 H158(0.5) C159(0.5) H159(0.5) C160(0.5) H160(0.5) N161(0.5) C190(0.5)
 C191(0.5) H191(0.5) C192(0.5) H192(0.5) C193(0.5) H193(0.5) C194(0.5)
 H194(0.5) N195(0.5) C196(0.5) C197(0.5) H197(0.5) C198(0.5) H198(0.5)
 C199(0.5) H199(0.5) C200(0.5) H200(0.5) N201(0.5) C184(0.5) C185(0.5)
 H185(0.5) C186(0.5) N187(0.5) C188(0.5) C189(0.5) H189(0.5) C172(0.5)
 C173(0.5) H173(0.5) C174(0.5) H174(0.5) C175(0.5) C176(0.5) H176(0.5)
 C177(0.5) H177(0.5) C178(0.5) C183(0.5) H183(0.5) C182(0.5) C181(0.5)
 H181(0.5) C180(0.5) H180(0.5) C179(0.5) H179(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C15(H15), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28),
  C29(H29), C30(H30), C37(H37), C36(H36), C34(H34), C33(H33), C39(H39),
 C41(H41), C42(H42), C43(H43), C45(H45), C49(H49), C51(H51), C52(H52), C53(H53),
  C54(H54), C57(H57), C58(H58), C59(H59), C60(H60), C63(H63), C64(H64),
 C66(H66), C67(H67), C69(H69), C70(H70), C71(H71), C73(H73), C75(H75), C79(H79),
  C81(H81), C82(H82), C83(H83), C84(H84), C87(H87), C88(H88), C89(H89),
 C90(H90), C93(H93), C94(H94), C96(H96), C97(H97), C99(H99), C100(H100),
 C101(H101), C103(H103), C105(H105), C109(H109), C111(H111), C112(H112),
 C113(H113), C114(H114), C117(H117), C118(H118), C119(H119), C120(H120),
 C137(H137), C136(H136), C134(H134), C133(H133), C143(H143), C141(H141),
 C140(H140), C139(H139), C149(H149), C145(H145), C151(H151), C152(H152),
 C153(H153), C154(H154), C157(H157), C158(H158), C159(H159), C160(H160),
 C191(H191), C192(H192), C193(H193), C194(H194), C197(H197), C198(H198),
 C199(H199), C200(H200), C185(H185), C189(H189), C173(H173), C174(H174),
 C176(H176), C177(H177), C183(H183), C181(H181), C180(H180), C179(H179)
6.b Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C8(C9,C10,C11,C12,C13), C14(C15,C16,N17,C18,C19), C20(C21,
 C22,C23,C24,N25), C26(C27,C28,C29,C30,N31), C32(C37,C36,C35,C34,C33), C38(C39,
 C40,C41,C42,C43), C44(C45,C46,N47,C48,C49), C50(C51,C52,C53,C54,N55), C56(C57,
 C58,C59,C60,N61), C62(C63,C64,C65,C66,C67), C68(C69,C70,C71,C72,C73), C74(C75,
 C76,N77,C78,C79), C80(C81,C82,C83,C84,N85), C86(C87,C88,C89,C90,N91), C92(C93,
 C94,C95,C96,C97), C98(C99,C100,C101,C102,C103), C104(C105,C106,N107,C108,C109),
  C110(C111,C112,C113,C114,N115), C116(C117,C118,C119,C120,N121), C132(C137,
 C136,C135,C134,C133), C138(C143,C142,C141,C140,C139), C144(C149,C148,N147,C146,
 C145), C150(C151,C152,C153,C154,N155), C156(C157,C158,C159,C160,N161),
 C190(C191,C192,C193,C194,N195), C196(C197,C198,C199,C200,N201), C184(C185,C186,
 N187,C188,C189), C172(C173,C174,C175,C176,C177), C178(C183,C182,C181,C180,C179)
;
_shelx_res_checksum              7982
_shelx_hkl_checksum              16111
_shelx_fab_checksum              52335
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'