Gallic acid-based dendrimers with a thiacalix[4]arene core: synthesis, aggregation and use for stabilization of Pd nanoparticles
Fatykhova, Aigul M.; Sultanova, Elza D.; Burilov, Vladimir A.; Gafiatullin, Bulat Kh.; Fedoseeva, Angelina A.; Veshta, Tatyana A.; Ziganshin, Marat A.; Ziganshina, Sufia A.; Evtugyn, Vladimir G.; Islamov, Daut R.; Usachev, Konstantin S.; Solovieva, Svetlana E.; Antipin, Igor S.; New Journal of Chemistry 47 (2023) 19223–19234; doi:10.1039/D3NJ03403H

data_7062767
_publ_section_title
;
 Gallic acid-based dendrimers with a thiacalix[4]arene core: synthesis,
 aggregation and use for stabilization of Pd nanoparticles
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19223
_journal_page_last               19234
_journal_paper_doi               10.1039/D3NJ03403H
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C60 H72 O8 S4'
_chemical_formula_sum            'C60 H72 O8 S4'
_chemical_formula_weight         1049.41
_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             2023-09-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2023-09-26 deposited with the CCDC.	2023-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.1600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3023(2)
_cell_length_b                   19.7017(2)
_cell_length_c                   19.7178(2)
_cell_measurement_reflns_used    25831
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      75.8740
_cell_measurement_theta_min      3.2240
_cell_volume                     5709.67(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_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    -35.00  25.00   0.50    1.00    --  -47.44  58.00-113.00  120
  2  \w   -117.00 -33.00   0.50    1.00    --  -47.44 -58.00 106.00  168
  3  \w    -11.00  20.00   0.50    1.00    --   47.44 -58.00 106.00   62
  4  \w     52.00  77.00   0.50    1.00    --   47.44  58.00-113.00   50
  5  \w    -59.00 -33.00   0.50    2.50    -- -106.00  58.00-113.00   52
  6  \w   -158.00-133.00   0.50    2.50    -- -106.00 -58.00 106.00   50
  7  \w     91.00 178.00   0.50    2.50    --  106.00  58.00-113.00  174
  8  \w     35.00  67.00   0.50    2.50    --  106.00 -58.00 106.00   64
  9  \w    -27.00  15.00   0.50    1.00    --   47.44 -19.00 120.00   84
 10  \w     14.00  92.00   0.50    1.00    --   47.44-125.00 -90.00  156
 11  \w    -27.00  24.00   0.50    1.00    --   47.44 -19.00 -60.00  102
 12  \w   -174.00-117.00   0.50    2.50    -- -106.00 -45.00-180.00  114
 13  \w   -112.00 -69.00   0.50    2.50    -- -106.00 125.00-120.00   86
 14  \w    -65.00 -36.00   0.50    2.50    -- -106.00  61.00-150.00   58
 15  \w    -70.00 -36.00   0.50    2.50    -- -106.00  61.00  30.00   68
 16  \w    -65.00 -36.00   0.50    2.50    -- -106.00  61.00   0.00   58
 17  \w     36.00  62.00   0.50    2.50    --  106.00 -61.00 -30.00   52
 18  \w     33.00  70.00   0.50    2.50    --  106.00 -61.00-120.00   74
 19  \w    132.00 174.00   0.50    2.50    --  106.00  61.00 150.00   84
 20  \w     33.00  98.00   0.50    2.50    --  106.00 -94.00-150.00  130
 21  \w     54.00 106.00   0.50    2.50    --  106.00 -94.00  60.00  104
 22  \w     34.00  78.00   0.50    2.50    --  106.00 -77.00  60.00   88
 23  \w     38.00  63.00   0.50    2.50    --  106.00 -61.00 150.00   50
 24  \w     97.00 165.00   0.50    2.50    --  106.00  45.00  30.00  136
 25  \w    101.00 127.00   0.50    2.50    --  106.00  61.00 150.00   52
 26  \w     35.00  63.00   0.50    2.50    --  106.00 -61.00 -90.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0593557000
_diffrn_orient_matrix_UB_12      -0.0541379000
_diffrn_orient_matrix_UB_13      -0.0477522000
_diffrn_orient_matrix_UB_21      0.0612465000
_diffrn_orient_matrix_UB_22      0.0036180000
_diffrn_orient_matrix_UB_23      -0.0500980000
_diffrn_orient_matrix_UB_31      0.0609709000
_diffrn_orient_matrix_UB_32      -0.0563057000
_diffrn_orient_matrix_UB_33      0.0426933000
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44220
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.764
_diffrn_reflns_theta_min         3.237
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.533
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.80a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.221
_exptl_crystal_description       needle
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         11619
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1128P)^2^+6.2575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10636
_reflns_number_total             11619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03403h2.cif
_cod_data_source_block           burv728_corr2
_cod_depositor_comments
'Adding full bibliography for 7062767--7062768.cif.'
_cod_database_code               7062767
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C60H70O8S4
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.602
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Restrained distances
 C15-C62 \\sim C62-C79
 with sigma of 0.001
 O28-C35 \\sim O4-C75
 with sigma of 0.001
 C59-C35 \\sim C75-C39
 with sigma of 0.001
 C7-O10 \\sim O6-C85
 with sigma of 0.001
 C31-C74 \\sim C74-C19
 with sigma of 0.001
 O10-C70 \\sim C70-O6
 with sigma of 0.001
 C33-C62 \\sim C62-C73
 with sigma of 0.001
 C2-C7 \\sim C85-C21
 with sigma of 0.001
 O4-C2 \\sim C21-O28
 with sigma of 0.001
 C71-C74 \\sim C74-C31
 with sigma of 0.001
 C5-C62 \\sim C62-C33
 with sigma of 0.001
 C81-C74 \\sim C74-C29
 with sigma of 0.001
 C29-C74 \\sim C74-C71
 with sigma of 0.001
 C79-C62 \\sim C62-C55
 with sigma of 0.001
 C55-C62 \\sim C62-C5
 with sigma of 0.001
 C17-C74 \\sim C74-C81
 with sigma of 0.001
 C77-C83 \\sim C57-C65
 with sigma of 0.001
 C37-C83 \\sim C57-C67
 with sigma of 0.001
 C37-O12 \\sim O20-C67
 with sigma of 0.001
 C63-C69 \\sim C41-C9
 with sigma of 0.001
 C41-O8 \\sim O8-C69
 with sigma of 0.001
 O20-C63 \\sim C9-O12
 with sigma of 0.001
 O28-C43 \\sim O4-C61
 with sigma of 0.001
 C61-C35 \\sim C75-C43
 with sigma of 0.001
 C59-C61 \\sim C43-C39
 with sigma of 0.001
 C11-C90 \\sim C90-C23
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C79)
Uanis(C63) = Uanis(C9)
Uanis(C65) = Uanis(C77)
Uanis(C55) = Uanis(C5)
Uanis(C69) = Uanis(C41)
Uanis(O12) = Uanis(O20)
Uanis(C37) = Uanis(C67)
Uanis(O10) = Uanis(O6)
Uanis(C19) = Uanis(C29)
Uanis(C39) = Uanis(C59)
Uanis(C23) = Uanis(C11)
4. Rigid body (RIGU) restrains
 C62, C15, C33, C55, C5, C73, C79
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O20, C57, C63, C65, C67, C69, O12, C9, C37, C41, C77, C83
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C74, C17, C29, C31, C19, C71, C81
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O4, O10, C2, C7, C35, C59, C61, O6, O28, C21, C39, C43, C75, C85
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=1-FVAR(2)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(2)
 Sof(O12)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=Sof(C77)=Sof(H77)=Sof(C83)=1-FVAR(3)
 Sof(O20)=Sof(C57)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C65)=Sof(H65)=Sof(C67)=
 Sof(H67A)=Sof(H67B)=Sof(C69)=Sof(H69A)=Sof(H69B)=FVAR(3)
 Sof(O6)=Sof(O28)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C39)=Sof(H39)=Sof(C43)=
 Sof(H43A)=Sof(H43B)=Sof(C75)=Sof(C85)=Sof(H85A)=Sof(H85B)=1-FVAR(4)
 Sof(O4)=Sof(O10)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C35)=
 Sof(C59)=Sof(H59)=Sof(C61)=Sof(H61A)=Sof(H61B)=FVAR(4)
 Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=Sof(C23)=Sof(C47)=Sof(H47A)=Sof(H47B)=
 Sof(H47C)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=1-FVAR(5)
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C11)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=FVAR(5)
6.a Free rotating group:
 C87(C11,C45,C89), C91(C23,C47,C93)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C13(H13A,H13B), C32(H32A,H32B), C49(H49A,H49B), C66(H66A,H66B),
 C92(H92A,H92B), C2(H2A,H2B), C7(H7A,H7B), C61(H61A,H61B), C63(H63A,H63B),
 C67(H67A,H67B), C69(H69A,H69B), C9(H9A,H9B), C21(H21A,H21B), C37(H37A,H37B),
 C41(H41A,H41B), C43(H43A,H43B), C85(H85A,H85B)
6.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C52(H52), C54(H54), C58(H58), C68(H68), C80(H80), C84(H84), C94(H94)
6.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C78(H78A,H78B,H78C), C82(H82A,H82B,H82C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C55(H55A,H55B,H55C), C87(H87A,H87B,H87C), C45(H45A,H45B,H45C),
 C89(H89A,H89B,H89C), C5(H5A,H5B,H5C), C19(H19A,H19B,H19C), C71(H71A,H71B,H71C),
  C73(H73A,H73B,H73C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C91(H91A,H91B,
 H91C), C47(H47A,H47B,H47C), C93(H93A,H93B,H93C)
6.e :
 C34(H34), C40(H40), C59(H59), C65(H65), C39(H39), C77(H77)
;
_shelx_res_checksum              11357
_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 1.528
_oxdiff_exptl_absorpt_empirical_full_min 0.722