Reticular synthesis of 8-connected carboxyl hydrogen-bonded organic frameworks for white-light-emission.
Xi, Xiao-Juan; Li, Yang; Lang, Feifan; Pang, Jiandong; Bu, Xian-He; Chemical science 15 (2024) 4529–4537; doi:10.1039/d3sc06410g

data_1571039
_publ_section_title
;
 Reticular synthesis of 8-connected carboxyl hydrogen-bonded organic
 frameworks for white-light-emission.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              4529
_journal_page_last               4537
_journal_paper_doi               10.1039/d3sc06410g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C98 H70 O18, 1.5(C16 H16 O4)'
_chemical_formula_sum            'C122 H94 O24'
_chemical_formula_weight         1943.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-30 deposited with the CCDC.	2024-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3338(5)
_cell_length_b                   25.9671(7)
_cell_length_c                   37.9645(8)
_cell_measurement_reflns_used    17408
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.6970
_cell_measurement_theta_min      2.3180
_cell_volume                     18074.0(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_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    -28.00  41.00   0.25    0.77    --   45.80 -36.00 -49.00  276
  2  \w   -173.00-126.00   0.25    3.07    -- -104.50 -87.00 160.00  188
  3  \w     40.00 101.00   0.25    3.07    --  105.14-125.00  88.00  244
  4  \w     90.00 150.00   0.25    3.07    --  105.14  36.00 107.00  240
  5  \w     55.00  80.00   0.25    3.07    --  105.14-146.00 -77.00  100
  6  \w    -23.00  29.00   0.25    0.77    --  -45.80  19.00-180.00  208
  7  \w    -19.00  22.00   0.25    0.77    --  -45.80  19.00  90.00  164
  8  \w    -20.00   6.00   0.25    0.77    --  -45.80  38.00-150.00  104
  9  \w     90.00 115.00   0.25    0.77    --   45.80 146.00 -27.00  100
 10  \w    -64.00 -39.00   0.25    3.07    -- -104.50  61.00 -60.00  100
 11  \w    -65.00 -34.00   0.25    3.07    -- -104.50  61.00 120.00  124
 12  \w     35.00 100.00   0.25    3.07    --  105.14-125.00-120.00  260
 13  \w     47.00 106.00   0.25    3.07    --  105.14 -77.00  90.00  236
 14  \w     39.00  74.00   0.25    3.07    --  105.14 -61.00 -30.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0581706000
_diffrn_orient_matrix_UB_12      0.0234751000
_diffrn_orient_matrix_UB_13      0.0244674000
_diffrn_orient_matrix_UB_21      -0.0475818000
_diffrn_orient_matrix_UB_22      0.0130599000
_diffrn_orient_matrix_UB_23      -0.0322545000
_diffrn_orient_matrix_UB_31      -0.0376205000
_diffrn_orient_matrix_UB_32      -0.0528664000
_diffrn_orient_matrix_UB_33      0.0028862000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            67768
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.836
_diffrn_reflns_theta_min         2.328
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.714
_exptl_crystal_description       block
_exptl_crystal_F_000             4072
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.382
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         18526
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.431
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.1155
_refine_ls_shift/su_max          0.006
_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          0.3421
_refine_ls_wR_factor_ref         0.3628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12240
_reflns_number_total             18526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06410g2.cif
_cod_data_source_block           nkm-hof-1
_cod_depositor_comments
'Adding full bibliography for 1571039--1571040.cif.'
_cod_database_code               1571039
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N'
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C31-C59
 1.39 with sigma of 0.01
 C63-C2
 1.54 with sigma of 0.01
 C29-C63 = C63-C2
 1.54 with sigma of 0.02
 C61-C65 = C65-C33
 1.54 with sigma of 0.02
 O13-C75
 1.43 with sigma of 0.01
 C59-C5
 1.39 with sigma of 0.005
 C29-C2
 2.515 with sigma of 0.04
 C61-C33
 2.515 with sigma of 0.04
 C61-C47 \\sim C65-C61 \\sim C33-C65
 with sigma of 0.01
 C57-C59 \\sim C31-C53 \\sim C15-C5
 with sigma of 0.01
 C15-C57 \\sim C57-C53 \\sim C53-C5 \\sim C59-C5 \\sim C31-C59 \\sim C31-C15
 with sigma of 0.01
 C29-C11 \\sim C63-C29 \\sim C63-C2
 with sigma of 0.01
3. Restrained planarity
 C57, C53, C5, C59, C31, C15
 with sigma of 0.1
4. Rigid bond restraints
 C47, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C63, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C11, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C23, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C65, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C37, O13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C47 \\sim C61: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C61 \\sim C65: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C75 \\sim O13: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C63 \\sim C2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C11 \\sim C29: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C29 \\sim C63: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C9 \\sim C71: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C37 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C65 \\sim C33: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C23 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C37 \\sim O13: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C59) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C75) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C73)
\\sim Ueq, Uanis(C69) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
6. Others
 Fixed Sof: H76A(0.5) H76B(0.5) H76C(0.5) H11A(0.5) H11B(0.5) H47A(0.5)
 H47B(0.5) H29A(0.5) H29B(0.5) H61A(0.5) H61B(0.5) C63(0.5) H63A(0.5) H63B(0.5)
 C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) H65A(0.5) H65B(0.5) H33A(0.5) H33B(0.5)
 H33C(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C17(0.5) C69(0.5) H69(0.5)
 C35(0.5) H35(0.5) C71(0.5) H71(0.5) C9(0.5) H9(0.5) C73(0.5) H73(0.5) C75(0.5)
 H75A(0.5) H75B(0.5) H75C(0.5)
7.a Riding coordinates:
 C76(H76A,H76B,H76C), C2(H2A,H2B,H2C), C33(H33A,H33B,H33C), C75(H75A,H75B,H75C)
7.b Ternary CH refined with riding coordinates:
 C12(H12A), C22(H22)
7.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C47(H47A,H47B), C29(H29A,H29B), C61(H61A,H61B), C63(H63A,
 H63B), C65(H65A,H65B)
7.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C28(H28), C30(H30), C36(H36), C42(H42), C46(H46), C54(H54),
 C58(H58), C60(H60), C62(H62), C64(H64), C66(H66), C72(H72), C39(H39), C21(H21),
  C45(H45), C49(H49), C25(H25), C51(H51), C13(H13), C53(H53), C27(H27),
 C55(H55), C7(H7A), C57(H57), C59(H59), C15(H15), C31(H31), C69(H69), C35(H35),
 C71(H71), C9(H9), C73(H73)
7.e Fitted hexagon refined as free rotating group:
 C17(C69,C35,C71,C9,C73)
7.f Tetrahedral OH refined with riding coordinates:
 O12(H12), O2(H2), O5(H5)
7.g Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C)
7.h Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37549
_shelx_fab_checksum              15199
_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 1.441
_oxdiff_exptl_absorpt_empirical_full_min 0.374