Supramolecular organogel formation behaviors of beads-on-string shaped poly(azomethine)s dependent on POSS structures in the main chains
Ishida, Ayano; Fujii, Shunichi; Sumida, Akifumi; Kamitani, Tasuku; Minami, Saori; Urayama, Kenji; Imoto, Hiroaki; Naka, Kensuke; Polymer Chemistry 12 (2021) 3169–3176; doi:10.1039/D1PY00346A

data_1562354
_publ_section_title
;
 Supramolecular organogel formation behaviors of beads-on-string shaped
 poly(azomethine)s dependent on POSS structures in the main chains
;
_journal_issue                   21
_journal_name_full               'Polymer Chemistry'
_journal_page_first              3169
_journal_page_last               3176
_journal_paper_doi               10.1039/D1PY00346A
_journal_volume                  12
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C56 H62 N2 O14 Si10'
_chemical_formula_sum            'C56 H62 N2 O14 Si10'
_chemical_formula_weight         1267.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-12 deposited with the CCDC.	2021-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0808(7)
_cell_length_b                   24.2770(15)
_cell_length_c                   25.8121(19)
_cell_measurement_reflns_used    3849
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      23.3890
_cell_measurement_theta_min      2.6520
_cell_volume                     6317.0(7)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB mini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20944
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.564
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 2379 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         12910
_refine_ls_number_restraints     513
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0934P)^2^+0.5919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1875
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7568
_reflns_number_total             12910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1py00346a2.cif
_cod_data_source_block           6
_cod_depositor_comments          'Adding full bibliography for 1562354.cif.'
_cod_database_code               1562354
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.914
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C70-C69
 1.54 with sigma of 0.02
 C71-C70
 1.54 with sigma of 0.02
 C71-N3
 1.47 with sigma of 0.02
 N2-C75
 1.47 with sigma of 0.02
 C74-C73
 1.54 with sigma of 0.02
 C75-C74
 1.54 with sigma of 0.02
3. Restrained planarity
 C30, C31, C32, C33, C34, C35
 with sigma of 0.1
 C52, C57, C56, C55, C54, C53
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C50 \\sim C40: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C41 \\sim C50: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C74 \\sim C70: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
N2 \\sim N3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C69 \\sim C74: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C71 \\sim C75: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C68 \\sim C72: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C60 \\sim C52: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C60 \\sim C58: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C59 \\sim C60: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C61 \\sim C52: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C21 \\sim C20: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C23 \\sim C17: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C21 \\sim C23: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
Si1 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C56 \\sim C60: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C61 \\sim C57: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C54 \\sim C58: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C59 \\sim C55: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C47 \\sim C41: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C51 \\sim C45: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C44 \\sim C50: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C42 \\sim C48: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C40 \\sim C46: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C43 \\sim C49: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C72 \\sim Si5: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C2 \\sim Si1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C72 \\sim C68: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.08 within 1.7A
C32 \\sim C37: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C39 \\sim C35: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C34 \\sim C38: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C36 \\sim C31: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C72) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C72) = Uanis(C68)
5. Rigid body (RIGU) restrains
 C40, C41, C42, C49, C50, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C72, Si5, C69, C70, C71, N3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C18, C19, C20, C21, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, C58, C53, C52, C61, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Si5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Si5, C73, C74, C75, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Si5, C69, C70, C71, N3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C30, C37, C36, C33, C39, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C36, C37, C33, C38, C39, C30
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C51, C46, C47, C48, C50, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C40, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C52, C53, C58, C59, C60, C61
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C23, C21, C20, C19, C18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, Si1, C2, C3, C4, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C52, C53, C54, C55, C56, C57
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C52, C61, C60, C59, C58, C53
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C72, Si5, C73, C74, C75, N2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C68, Si5, C69, C70, C71, N3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C30, C31, C32, C33, C38, C39
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C30, C36, C37, C33, C34, C35
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Si1, C2, C3, C4, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C31, C30, C35, C34, C33, C32
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C30, C35, C34, C33, C32, C31
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C32, C33, C34, C35, C30, C31
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C69)=Sof(H69a)=Sof(H69b)=Sof(C70)=Sof(H70a)=Sof(H70b)=Sof(C71)=Sof(H71a)=
 Sof(H71b)=Sof(N3)=Sof(H3c)=Sof(H3d)=Sof(C68)=Sof(H68a)=Sof(H68b)=Sof(H68c)=1-
 FVAR(1)
 Sof(C72)=Sof(H72a)=Sof(H72b)=Sof(H72c)=Sof(N2)=Sof(H2c)=Sof(H2d)=Sof(C75)=
 Sof(H75a)=Sof(H75b)=Sof(C74)=Sof(H74a)=Sof(H74b)=Sof(C73)=Sof(H73a)=Sof(H73b)=
 FVAR(1)
 Sof(C40)=Sof(C45)=Sof(H45)=Sof(C44)=Sof(H44)=Sof(C43)=Sof(H43)=Sof(C42)=
 Sof(H42)=Sof(C41)=Sof(H41)=1-FVAR(2)
 Sof(C46)=Sof(C51)=Sof(H51)=Sof(C50)=Sof(H50)=Sof(C49)=Sof(H49)=Sof(C48)=
 Sof(H48)=Sof(C47)=Sof(H47)=FVAR(2)
 Sof(H53a)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=Sof(C61)=
 Sof(H61)=1-FVAR(3)
 Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(C57)=
 Sof(H57)=FVAR(3)
 Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(H33)=Sof(C38)=Sof(H38)=Sof(C39)=
 Sof(H39)=1-FVAR(4)
 Sof(H33a)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C34)=Sof(H34)=Sof(C35)=
 Sof(H35)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C69(H69a,H69b), C70(H70a,H70b),
 C71(H71a,H71b), C75(H75a,H75b), C74(H74a,H74b), C73(H73a,H73b)
7.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C67(H67), C66(H66),
 C65(H65), C64(H64), C63(H63), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
  C9(H9), C25(H25), C10(H10), C7(H7), C45(H45), C44(H44), C43(H43), C42(H42),
 C41(H41), C29(H29), C6(H6), C8(H8), C26(H26), C27(H27), C28(H28), C53(H53),
 C53(H53a), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C61(H61), C36(H36), C37(H37), C33(H33), C33(H33a), C38(H38),
 C39(H39), C31(H31), C32(H32), C34(H34), C35(H35), C51(H51), C50(H50), C49(H49),
  C48(H48), C47(H47)
7.c Fitted hexagon refined as free rotating group:
 C11(C12,C13,C14,C15,C16), C62(C67,C66,C65,C64,C63), C17(C18,C19,C20,C21,C23),
 C40(C45,C44,C43,C42,C41), C52(C53,C54,C55,C56,C57), C30(C36,C37,C33,C38,C39),
 C46(C51,C50,C49,C48,C47)
7.d X=CH2 refined with riding coordinates:
 N1(H1d,H1e), N3(H3c,H3d), N2(H2c,H2d)
7.e Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C72(H72a,H72b,H72c), C68(H68a,H68b,H68c)
;
_shelx_res_checksum              36170
_olex2_submission_special_instructions 'No special instructions were received'