Modularly prepared segmented fluorinated silicones and their anomalous microstructure dependent flow behavior.
Migliaccio, Analise C.; Weeks, Nathan J.; Iacono, Scott T.; RSC advances 15 (2025) 21429–21438; doi:10.1039/d5ra03087k

data_7250600
_publ_section_title
;
 Modularly prepared segmented fluorinated silicones and their anomalous
 microstructure dependent flow behavior.
;
_journal_issue                   27
_journal_name_full               'RSC advances'
_journal_page_first              21429
_journal_page_last               21438
_journal_paper_doi               10.1039/d5ra03087k
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C36 H26 F12 O6'
_chemical_formula_sum            'C36 H26 F12 O6'
_chemical_formula_weight         782.57
_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_block_doi                 10.5517/ccdc.csd.cc2mx9mh
_audit_creation_date             2025-04-01
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.6970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.94960(10)
_cell_length_b                   8.82620(10)
_cell_length_c                   18.0438(2)
_cell_measurement_reflns_used    22671
_cell_measurement_temperature    104(6)
_cell_measurement_theta_max      68.8070
_cell_measurement_theta_min      2.5330
_cell_volume                     1670.29(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -30.00  24.00   0.50    0.20    --   43.05 -11.00-180.00  108
  2  \w    -22.00  37.00   0.50    0.20    --   43.05 -32.00 -30.00  118
  3  \w    -22.00  61.00   0.50    0.20    --   43.05 -58.00  27.00  166
  4  \w    -22.00  37.00   0.50    0.20    --   43.05 -32.00 120.00  118
  5  \w     46.00  99.00   0.50    0.20    --   94.32 -77.00  90.00  106
  6  \w     30.00  66.00   0.50    0.20    --   94.32 -59.00 -60.00   72
  7  \w     28.00  54.00   0.50    0.20    --   94.32 -77.00 -90.00   52
  8  \w     56.00  82.00   0.50    0.20    --   94.32 -68.00-180.00   52
  9  \w     31.00  80.00   0.50    0.20    --   94.32 -68.00-120.00   98
 10  \w     28.00  68.00   0.50    0.20    --   94.32 -59.00 -90.00   80
 11  \w     68.00 106.00   0.50    0.20    --   94.32 -77.00 -90.00   76
 12  \w     30.00  55.00   0.50    0.20    --   94.32 -50.00 -90.00   50
 13  \w     29.00  54.00   0.50    0.20    --   94.32 -50.00 -60.00   50
 14  \w     29.00  57.00   0.50    0.20    --   94.32 -50.00   0.00   56
 15  \w     28.00  67.00   0.50    0.20    --   94.32 -58.00  27.00   78
 16  \w     28.00  68.00   0.50    0.20    --   94.32 -59.00 120.00   80
 17  \w     29.00  57.00   0.50    0.20    --   94.32 -50.00 150.00   56
 18  \w     44.00 127.00   0.50    0.20    --   94.32-145.00 -90.00  166
 19  \w     44.00 127.00   0.50    0.20    --   94.32-145.00 -90.00  166
 20  \w     33.00 110.00   0.50    0.20    --   94.32-117.00 -90.00  154
 21  \w     33.00 110.00   0.50    0.20    --   94.32-117.00 -90.00  154
 22  \w     33.00 110.00   0.50    0.20    --   94.32-117.00  30.00  154
 23  \w     96.00 127.00   0.50    0.20    --   94.32-145.00  30.00   62
 24  \w     64.00 110.00   0.50    0.20    --   94.32-117.00  90.00   92
 25  \w     33.00 110.00   0.50    0.20    --   94.32-117.00 150.00  154
 26  \w     33.00 110.00   0.50    0.20    --   94.32-117.00 150.00  154
 27  \w     51.00  84.00   0.50    0.20    --   94.32-145.00 150.00   66
 28  \w     26.00 107.00   0.50    0.20    --   94.32 -96.00  90.00  162
 29  \w     26.00 107.00   0.50    0.20    --   94.32 -96.00  60.00  162
 30  \w     26.00 107.00   0.50    0.20    --   94.32 -96.00  30.00  162
 31  \w     27.00 122.00   0.50    0.20    --   94.32 -86.00-120.00  190
 32  \w     28.00  86.00   0.50    0.20    --   94.32 -96.00-180.00  116
 33  \w     18.00  78.00   0.50    0.20    --   43.05-104.00-150.00  120
 34  \w     41.00  99.00   0.50    0.20    --   43.05-138.00  60.00  116
 35  \w     41.00  99.00   0.50    0.20    --   43.05-138.00  90.00  116
 36  \w     25.00 110.00   0.50    0.20    --   43.05  58.00 168.00  170
 37  \w     76.00 161.00   0.50    0.20    --   94.32  58.00 168.00  170
 38  \w     76.00 161.00   0.50    0.20    --   94.32  58.00 168.00  170
 39  \w     76.00 161.00   0.50    0.20    --   94.32  59.00-180.00  170
 40  \w     76.00 161.00   0.50    0.20    --   94.32  59.00-180.00  170
 41  \w     79.00 160.00   0.50    0.20    --   94.32  50.00-120.00  162
 42  \w     79.00 160.00   0.50    0.20    --   94.32  50.00-120.00  162
 43  \w     86.00 159.00   0.50    0.20    --   94.32  33.00-150.00  146
 44  \w     86.00 159.00   0.50    0.20    --   94.32  33.00 -90.00  146
 45  \w     88.00 162.00   0.50    0.20    --   94.32  25.00  30.00  148
 46  \w     84.00 165.00   0.50    0.20    --   94.32  17.00 -30.00  162
 47  \w     88.00 162.00   0.50    0.20    --   94.32  25.00  90.00  148
 48  \w     79.00 160.00   0.50    0.20    --   94.32  50.00 120.00  162
 49  \w     86.00 159.00   0.50    0.20    --   94.32  33.00 150.00  146
 50  \w    132.00 158.00   0.50    0.20    --   94.32  25.00  90.00   52
 51  \w     84.00 164.00   0.50    0.20    --   94.32  17.00   0.00  160
 52  \w    -24.00  30.00   0.50    0.20    --  -43.05  11.00 -60.00  108
 53  \w    -28.00  26.00   0.50    0.20    --  -43.05  21.00   0.00  108
 54  \w    -61.00  23.00   0.50    0.20    --  -43.05  58.00 168.00  168
 55  \w    -61.00  23.00   0.50    0.20    --  -43.05  58.00 168.00  168
 56  \w    -67.00 -14.00   0.50    0.20    --  -80.25  58.00 168.00  106
 57  \w    -47.00 -15.00   0.50    0.20    --  -80.25  42.00  60.00   64
 58  \w    -47.00 -15.00   0.50    0.20    --  -80.25  42.00   0.00   64
 59  \w    -47.00 -15.00   0.50    0.20    --  -80.25  42.00 -30.00   64
 60  \w    -47.00 -15.00   0.50    0.20    --  -80.25  42.00 -60.00   64
 61  \w    -47.00 -15.00   0.50    0.20    --  -80.25  42.00 -90.00   64
 62  \w    -47.00 -15.00   0.50    0.20    --  -80.25  42.00 120.00   64
 63  \w   -112.00 -35.00   0.50    0.20    --  -43.05 -21.00  30.00  154
 64  \w   -110.00 -19.00   0.50    0.20    --  -43.05 -77.00 -30.00  182
 65  \w   -110.00 -19.00   0.50    0.20    --  -43.05 -77.00 -30.00  182
 66  \w   -109.00 -23.00   0.50    0.20    --  -43.05 -65.00 -30.00  172
 67  \w   -108.00 -25.00   0.50    0.20    --  -43.05 -58.00  27.00  166
 68  \w   -108.00 -25.00   0.50    0.20    --  -43.05 -58.00  27.00  166
 69  \w    -96.00 -19.00   0.50    0.20    --  -43.05 138.00 -90.00  154
 70  \w    -96.00 -19.00   0.50    0.20    --  -43.05 138.00 -90.00  154
 71  \w   -112.00 -35.00   0.50    0.20    --  -43.05 -21.00  30.00  154
 72  \w   -146.00 -62.00   0.50    0.20    --  -80.25 -58.00  27.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1304753000
_diffrn_orient_matrix_UB_12      -0.0755132000
_diffrn_orient_matrix_UB_13      -0.0095040000
_diffrn_orient_matrix_UB_21      -0.0252534000
_diffrn_orient_matrix_UB_22      0.1093355000
_diffrn_orient_matrix_UB_23      0.0605196000
_diffrn_orient_matrix_UB_31      -0.0627106000
_diffrn_orient_matrix_UB_32      0.1131610000
_diffrn_orient_matrix_UB_33      -0.0647240000
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31045
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.977
_diffrn_reflns_theta_min         4.256
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.297
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             796
_exptl_crystal_recrystallization_method 'Recrystallized from hexane'
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0465P)^2^+0.8167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2925
_reflns_number_total             3091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03087k2.cif
_cod_data_source_block           benzpfcpdieugabs
_cod_database_code               7250600
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C36 H26 F12 O6'
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.671
_diffrn_oxdiff_ac3_digest_hkl    4181d666b0bbb7fc46fc43a94dd6d066d2a6c0
_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.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C11(H11), C13(H13), C14(H14), C16(H16)
2.c X=CH2 refined with riding coordinates:
 C17(H17A,H17B)
2.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_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 2.362
_oxdiff_exptl_absorpt_empirical_full_min 0.703