Reversible hydrogen-bonded polymerization regulated by allosteric metal templation.
Xiao, Tangxin; Zhong, Weiwei; Yang, Weiwei; Qi, Lijie; Gao, Yan; Sue, Andrew C.-H.; Li, Zheng-Yi; Sun, Xiao-Qiang; Lin, Chen; Wang, Leyong; Chemical communications (Cambridge, England) 56 (2020) 14385–14388; doi:10.1039/d0cc06381a

data_7127752
_publ_section_title
;
 Reversible hydrogen-bonded polymerization regulated by allosteric metal
 templation.
;
_journal_issue                   92
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14385
_journal_page_last               14388
_journal_paper_doi               10.1039/d0cc06381a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C64 H92 F12 K2 N16 O16 P2'
_chemical_formula_sum            'C64 H92 F12 K2 N16 O16 P2'
_chemical_formula_weight         1709.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-01 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.689(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5377(3)
_cell_length_b                   16.9875(3)
_cell_length_c                   31.4097(5)
_cell_measurement_reflns_used    33484
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      30.2240
_cell_measurement_theta_min      2.2680
_cell_volume                     7748.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -48.00  61.00   0.50   11.01    --  -13.65  78.00 -73.00  218
  2  \w     39.00  97.00   0.50   11.01    --   12.17 178.00 120.00  116
  3  \w    -63.00  29.00   0.50   11.01    --   12.17 -57.00 -30.00  184
  4  \w    -22.00   9.00   0.50   11.01    --  -13.65 -99.00  30.00   62
  5  \w     36.00  98.00   0.50   11.01    --   12.17-178.00 150.00  124
  6  \w    -88.00  21.00   0.50   11.01    --  -13.65 -78.00 162.00  218
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0193747000
_diffrn_orient_matrix_UB_12      -0.0252477000
_diffrn_orient_matrix_UB_13      0.0151691000
_diffrn_orient_matrix_UB_21      -0.0174429000
_diffrn_orient_matrix_UB_22      -0.0247346000
_diffrn_orient_matrix_UB_23      -0.0167076000
_diffrn_orient_matrix_UB_31      0.0413012000
_diffrn_orient_matrix_UB_32      -0.0222430000
_diffrn_orient_matrix_UB_33      0.0013566000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            89268
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.169
_diffrn_reflns_theta_min         1.845
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light colourless'
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         18989
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0819P)^2^+2.6556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12945
_reflns_number_total             18989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06381a2.cif
_cod_data_source_block           yww-czu-1a
_cod_database_code               7127752
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.936
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C43 \\sim O1-C43A
 with sigma of 0.02
 C42-C43 \\sim C42-C43A
 with sigma of 0.02
 C62-C63 \\sim C62-C63A
 with sigma of 0.02
 C63-C64 \\sim C63A-C64A
 with sigma of 0.02
 C62-C64 \\sim C62-C64A
 with sigma of 0.04
 C27-C28 \\sim C27-C28A
 with sigma of 0.02
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
 C37-C38 \\sim C37-C38A
 with sigma of 0.02
 C39-C38 \\sim C39A-C38A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 C37-C39 \\sim C37-C39A
 with sigma of 0.04
 C38-C40 \\sim C38A-C40A
 with sigma of 0.04
 O15-C11 \\sim O15-C11A
 with sigma of 0.02
 C10-C11 \\sim C10-C11A
 with sigma of 0.02
 C5-C6 \\sim C5-C6A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 C5-C7 \\sim C5-C7A
 with sigma of 0.04
 C28-C29 \\sim C28A-C29A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C27-C29 \\sim C27-C29A
 with sigma of 0.04
 C3-C5 \\sim C5-C6A \\sim C6A-C7A \\sim C7A-C8A
 with sigma of 0.01
 C8-C7 \\sim C8A-C7A
 with sigma of 0.02
 C6-C8 \\sim C6A-C8A
 with sigma of 0.04
 C35-C37 \\sim C37-C38A \\sim C38A-C39A
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C37, C38A, C38, C39A, C39, C40, C40A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C27, C28, C28A, C29A, C30A, C30, C29
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C5, C6, C6A, C7, C7A, C8A, C8
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=1-FVAR(1)
 Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(1)
 Sof(H62C)=Sof(H62D)=Sof(C63A)=Sof(H63C)=Sof(H63D)=Sof(C64A)=Sof(H64D)=
 Sof(H64E)=Sof(H64F)=1-FVAR(2)
 Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=Sof(H64B)=
 Sof(H64C)=FVAR(2)
 Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=
 Sof(H29D)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(3)
 Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(3)
 Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=
 Sof(H39D)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(4)
 Sof(H37A)=Sof(H37B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(4)
 Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=1-FVAR(5)
 Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(5)
 Sof(H5BC)=Sof(H5BD)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(6)
 Sof(H5AA)=Sof(H5AB)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(6)
5.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C21(H21A,H21B), C54(H54A,H54B), C53(H53A,H53B), C20(H20A,
 H20B), C42(H42A,H42B), C42(H42C,H42D), C10(H10A,H10B), C10(H10C,H10D),
 C52(H52A,H52B), C61(H61A,H61B), C23(H23A,H23B), C27(H27A,H27B), C27(H27C,H27D),
  C55(H55A,H55B), C45(H45A,H45B), C13(H13A,H13B), C12(H12A,H12B), C44(H44A,
 H44B), C62(H62A,H62B), C62(H62C,H62D), C11(H11A,H11B), C28(H28A,H28B),
 C37(H37A,H37B), C37(H37C,H37D), C5(H5AA,H5AB), C5(H5BC,H5BD), C29(H29A,H29B),
 C63(H63A,H63B), C39(H39A,H39B), C38(H38A,H38B), C43(H43A,H43B), C6(H6A,H6B),
 C7(H7A,H7B), C43A(H43C,H43D), C63A(H63C,H63D), C28A(H28C,H28D), C29A(H29C,
 H29D), C38A(H38C,H38D), C39A(H39C,H39D), C11A(H11C,H11D), C6A(H6AA,H6AB),
 C7A(H7AA,H7AB)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N14(H14), N7(H7), N10(H10), N1(H1), N0AA(H0AA), N9(H9),
 N13(H13), N5(H5), N11(H11), N4(H4), C59(H59), C31(H31), C18(H18), C34(H34),
 C50(H50), C15(H15), C47(H47), C2(H2), C16(H16), C49(H49), C17(H17), C48(H48)
5.c Idealised Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C64(H64A,H64B,H64C), C40(H40A,H40B,H40C), C64A(H64D,H64E,
 H64F), C30A(H30D,H30E,H30F), C40A(H40D,H40E,H40F)
;
_shelx_res_checksum              84239
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.738