Self-assembled sonogels formed from 1,4-naphthalenedicarbonyldinicotinic acid hydrazide
Liao, Lieqiang; Liu, Ruidong; Hu, Shuwen; Jiang, Wenting; Chen, Yali; Zhong, Jinlian; Jia, Xinjian; Liu, Huijin; Luo, Xuzhong; RSC Advances 12 (2022) 20218–20226; doi:10.1039/D2RA01391F

data_7245212
_publ_section_title
;
 Self-assembled sonogels formed from 1,4-naphthalenedicarbonyldinicotinic
 acid hydrazide
;
_journal_issue                   31
_journal_name_full               'RSC Advances'
_journal_page_first              20218
_journal_page_last               20226
_journal_paper_doi               10.1039/D2RA01391F
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         '4(C24 H18 N6 O4), 6(H2 O), 3(C2 H6 O)'
_chemical_formula_sum            'C102 H102 N24 O25'
_chemical_formula_weight         2064.07
_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   mixed
_audit_creation_date             2020-09-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-15 deposited with the CCDC.	2022-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.440(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   8.0569(2)
_cell_length_b                   36.1507(7)
_cell_length_c                   8.9337(2)
_cell_measurement_reflns_used    5202
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      78.4380
_cell_measurement_theta_min      4.8600
_cell_volume                     2601.98(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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     -1.00  24.00   0.50    0.80    --    0.00  20.00  73.00   50
  2  \w     58.00  83.00   0.50    3.19    --  105.20 -20.00 -93.00   50
  3  \w    110.00 146.00   0.50    3.19    --  105.20  20.00  73.00   72
  4  \w    -23.00   3.00   0.50    0.80    --    0.00 -57.00-180.00   52
  5  \w    -32.00  84.00   0.50    0.80    --    0.00  77.00 -60.00  232
  6  \w     90.00 123.00   0.50    3.19    --  105.20 -30.00  60.00   66
  7  \w     16.00  78.00   0.50    3.19    --  105.20 -30.00  60.00  124
  8  \w     77.00 126.00   0.50    3.19    --  105.20 -82.00  90.00   98
  9  \w     67.00 124.00   0.50    3.19    --  105.20 -45.00  60.00  114
 10  \w     16.00 132.00   0.50    3.19    --  105.20 -30.00 -60.00  232
 11  \w    134.00 159.00   0.50    3.19    --  105.20  45.00-120.00   50
 12  \w     82.00 107.00   0.50    3.19    --  105.20 -82.00 120.00   50
 13  \w     22.00 115.00   0.50    3.19    --  105.20 -61.00 150.00  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0499705000
_diffrn_orient_matrix_UB_12      0.0410711000
_diffrn_orient_matrix_UB_13      0.0088163000
_diffrn_orient_matrix_UB_21      0.0081518000
_diffrn_orient_matrix_UB_22      -0.0017076000
_diffrn_orient_matrix_UB_23      0.1720624000
_diffrn_orient_matrix_UB_31      0.1844885000
_diffrn_orient_matrix_UB_32      0.0112238000
_diffrn_orient_matrix_UB_33      -0.0036375000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11781
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        66.496
_diffrn_reflns_theta_max         66.496
_diffrn_reflns_theta_min         4.893
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1082
_exptl_crystal_recrystallization_method
'gel formed from compounds in ethanol gradually transformed into granular crystals upon extension of the aging time'
_exptl_crystal_size_max          0.513
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.235
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4415
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.1023
_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^)+(0.1784P)^2^+4.1912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2832
_refine_ls_wR_factor_ref         0.2949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3708
_reflns_number_total             4415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra01391f2.cif
_cod_data_source_block           l-1
_cod_database_code               7245212
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.682
_reflns_odcompleteness_completeness 93.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H1-H22
 2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim N5 \\sim C26 \\sim C24 \\sim C25: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: O5(0.75) H5A(0.75) H5B(0.75) O8(0.75) H8(0.75) O6(0.75) H6A(0.75)
 H6B(0.75) C27(0.75) H27A(0.75) H27B(0.75) C28(0.75) H28A(0.75) H28B(0.75)
 H28C(0.75)
5.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
5.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C3(H3A), C5(H5), C6(H6), C9(H9), C12(H12), C13(H13), C14(H14),
  N2(H2), C16(H16), C17(H17), C18(H18), N1(H1), C22(H22), C24(H24), C25(H25),
 C26(H26)
5.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C)
5.e Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              97148
_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 3.468
_oxdiff_exptl_absorpt_empirical_full_min 0.449