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_1571040
_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         'C92 H58 O18, 1.5(C16 H16 O4)'
_chemical_formula_sum            'C116 H82 O24'
_chemical_formula_weight         1859.81
_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                   18.3974(3)
_cell_length_b                   26.3784(3)
_cell_length_c                   37.7312(4)
_cell_measurement_reflns_used    23187
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      75.0890
_cell_measurement_theta_min      2.1480
_cell_volume                     18310.7(4)
_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      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_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     33.00  59.00   0.50    2.97    --  105.14 -61.00-150.00   52
  2  \w     48.00  93.00   0.50    0.74    --   46.05-125.00 -30.00   90
  3  \w     39.00  75.00   0.50    2.97    --  105.14 -61.00 120.00   72
  4  \w     93.00 158.00   0.50    2.97    --  105.14  29.00-102.00  130
  5  \w    108.00 178.00   0.50    2.97    --  105.14  95.00  70.00  140
  6  \w    -18.00  38.00   0.50    0.74    --   46.05 -29.00  96.00  112
  7  \w    -19.00  28.00   0.50    0.74    --  -46.05  19.00 -30.00   94
  8  \w     -7.00  27.00   0.50    0.74    --  -46.05  19.00  60.00   68
  9  \w    -62.00 -34.00   0.50    2.97    -- -104.50  61.00  90.00   56
 10  \w    -66.00 -40.00   0.50    2.97    -- -104.50  61.00-120.00   52
 11  \w    -10.00  15.00   0.50    0.74    --  -46.05  19.00-180.00   50
 12  \w   -101.00 -34.00   0.50    2.97    -- -104.50 125.00 -60.00  134
 13  \w   -168.00 -80.00   0.50    2.97    -- -104.50-120.00-118.00  176
;
_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      0.0750626000
_diffrn_orient_matrix_UB_12      -0.0219598000
_diffrn_orient_matrix_UB_13      -0.0095896000
_diffrn_orient_matrix_UB_21      0.0217827000
_diffrn_orient_matrix_UB_22      0.0012853000
_diffrn_orient_matrix_UB_23      0.0394227000
_diffrn_orient_matrix_UB_31      -0.0298692000
_diffrn_orient_matrix_UB_32      -0.0541158000
_diffrn_orient_matrix_UB_33      0.0047719000
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            71805
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.272
_diffrn_reflns_theta_min         2.044
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82533
_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    0.675
_exptl_crystal_description       block
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.361
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         18813
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.390
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.1085
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3230
_refine_ls_wR_factor_ref         0.3410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13143
_reflns_number_total             18813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06410g2.cif
_cod_data_source_block           nkm-hof-2
_cod_depositor_comments
'Adding full bibliography for 1571039--1571040.cif.'
_cod_database_code               1571040
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O'
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.892
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C31-C15
 1.395 with sigma of 0.005
 C61_$1-C27
 1.395 with sigma of 0.005
 C59-C53
 1.395 with sigma of 0.01
 C27-C15 \\sim C61-C31_$1 \\sim C31-C61_$1
 with sigma of 0.01
 C59-C53 \\sim C53-C5 \\sim C63-C5 \\sim C65-C63 \\sim C65-C2 \\sim C59-C2
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C65) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H44A(0.5) H44B(0.5) H44C(0.5) H60A(0.5) H60B(0.5) H60C(0.5)
 H64A(0.5) H64B(0.5) H64C(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C67(0.5)
 H67A(0.5) H67B(0.5) H67C(0.5)
5.a Riding coordinates:
 C44(H44A,H44B,H44C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C)
5.b Ternary CH refined with riding coordinates:
 C6(H6), C28(H28)
5.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C24(H24), C30(H30), C32(H32), C46(H46), C48(H48), C54(H54),
 C62(H62), C66(H66), C68(H68), C17(H17), C37(H37), C39(H39), C41(H41), C43(H43),
  C11(H11A), C45(H45), C3(H3), C25(H25), C13(H13), C53(H53), C55(H55), C7(H7A),
 C57(H57), C59(H59), C15(H15), C61(H61), C31(H31), C63(H63), C2(H2), C65(H65)
5.d Tetrahedral OH refined with riding coordinates:
 O8(H8), O11(H11)
5.e Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C67(H67A,H67B,H67C)
5.f Idealised tetrahedral OH refined as rotating group:
 O7(H7), O5(H5)
;
_shelx_res_checksum              64156
_shelx_fab_checksum              84473
_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 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.605