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_7250599
_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         'C25 H22 F6 O4'
_chemical_formula_sum            'C25 H22 F6 O4'
_chemical_formula_weight         500.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2mx93z
_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                 94.1900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.34020(10)
_cell_length_b                   23.04830(10)
_cell_length_c                   8.64280(10)
_cell_measurement_reflns_used    30411
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      68.7110
_cell_measurement_theta_min      3.8230
_cell_volume                     2252.95(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      100.0(2)
_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 0.997
_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    -22.00  48.00   0.50    0.20    --   42.38 -43.00 120.00  140
  2  \w    -23.00  37.00   0.50    0.20    --   42.38 -32.00  30.00  120
  3  \w    -31.00  24.00   0.50    0.20    --   42.38 -11.00 -30.00  110
  4  \w     28.00  83.00   0.50    0.20    --   94.43 -68.00 -60.00  110
  5  \w     28.00  83.00   0.50    0.20    --   94.43 -68.00-120.00  110
  6  \w     26.00 106.00   0.50    0.20    --   94.43 -77.00-150.00  160
  7  \w     26.00 106.00   0.50    0.20    --   94.43 -77.00-150.00  160
  8  \w     28.00  83.00   0.50    0.20    --   94.43 -68.00-180.00  110
  9  \w     28.00  68.00   0.50    0.20    --   94.43 -59.00 -30.00   80
 10  \w     28.00  57.00   0.50    0.20    --   94.43 -50.00-120.00   58
 11  \w     28.00  68.00   0.50    0.20    --   94.43 -59.00  60.00   80
 12  \w     28.00  57.00   0.50    0.20    --   94.43 -50.00  60.00   58
 13  \w     28.00  57.00   0.50    0.20    --   94.43 -50.00  90.00   58
 14  \w     28.00  57.00   0.50    0.20    --   94.43 -50.00 120.00   58
 15  \w    -22.00  69.00   0.50    0.20    --   42.38 -83.00  60.00  182
 16  \w     44.00 126.00   0.50    0.20    --   94.43-144.00  60.00  164
 17  \w     33.00 110.00   0.50    0.20    --   94.43-117.00  60.00  154
 18  \w     44.00 126.00   0.50    0.20    --   94.43-144.00  60.00  164
 19  \w     33.00 110.00   0.50    0.20    --   94.43-117.00 -30.00  154
 20  \w     33.00 110.00   0.50    0.20    --   94.43-117.00 -30.00  154
 21  \w     44.00 126.00   0.50    0.20    --   94.43-144.00-120.00  164
 22  \w     33.00 110.00   0.50    0.20    --   94.43-117.00 -90.00  154
 23  \w     33.00 110.00   0.50    0.20    --   94.43-117.00-180.00  154
 24  \w     18.00  78.00   0.50    0.20    --   42.38-104.00 -60.00  120
 25  \w     25.00 106.00   0.50    0.20    --   94.43 -96.00  60.00  162
 26  \w     25.00 106.00   0.50    0.20    --   94.43 -96.00  60.00  162
 27  \w     26.00 123.00   0.50    0.20    --   94.43 -86.00 120.00  194
 28  \w     26.00 123.00   0.50    0.20    --   94.43 -86.00 120.00  194
 29  \w     26.00 121.00   0.50    0.20    --   94.43 -83.00  60.00  190
 30  \w     26.00 123.00   0.50    0.20    --   94.43 -86.00 -60.00  194
 31  \w    -37.00  23.00   0.50    0.20    --  -42.38  32.00   0.00  120
 32  \w    -24.00  32.00   0.50    0.20    --  -42.38  11.00 -30.00  112
 33  \w    -28.00  27.00   0.50    0.20    --  -42.38  21.00 -60.00  110
 34  \w    -24.00  32.00   0.50    0.20    --  -42.38  11.00-180.00  112
 35  \w    -84.00 -18.00   0.50    0.20    --  -80.25 117.00-120.00  132
 36  \w    -69.00  26.00   0.50    0.20    --  -42.38  83.00-178.00  190
 37  \w    -69.00  26.00   0.50    0.20    --  -42.38  83.00-178.00  190
 38  \w   -107.00 -11.00   0.50    0.20    --  -80.25  83.00-178.00  192
 39  \w   -107.00 -11.00   0.50    0.20    --  -80.25  83.00-178.00  192
 40  \w    -47.00 -14.00   0.50    0.20    --  -80.25  42.00 -90.00   66
 41  \w    -47.00 -14.00   0.50    0.20    --  -80.25  42.00-150.00   66
 42  \w    -57.00 -14.00   0.50    0.20    --  -80.25  50.00  30.00   86
 43  \w    -47.00 -14.00   0.50    0.20    --  -80.25  42.00  60.00   66
 44  \w   -110.00 -17.00   0.50    0.20    --  -42.38 -77.00  30.00  186
 45  \w   -148.00 -78.00   0.50    0.20    --  -80.25 -83.00  60.00  140
 46  \w   -148.00 -78.00   0.50    0.20    --  -80.25 -86.00 120.00  140
 47  \w   -109.00 -64.00   0.50    0.20    --  -42.38-138.00 -90.00   90
 48  \w     33.00 108.00   0.50    0.20    --   42.38  32.00 -30.00  150
 49  \w     72.00 161.00   0.50    0.20    --   94.43  68.00-150.00  178
 50  \w     21.00 109.00   0.50    0.20    --   42.38  65.00-180.00  176
 51  \w     84.00 160.00   0.50    0.20    --   94.43  33.00 -90.00  152
 52  \w     33.00 108.00   0.50    0.20    --   42.38  32.00 -30.00  150
 53  \w     75.00 160.00   0.50    0.20    --   94.43  59.00  90.00  170
 54  \w     81.00 159.00   0.50    0.20    --   94.43  42.00 150.00  156
 55  \w     86.00 162.00   0.50    0.20    --   94.43  25.00  90.00  152
 56  \w     84.00 160.00   0.50    0.20    --   94.43  33.00   0.00  152
 57  \w     86.00 162.00   0.50    0.20    --   94.43  25.00-120.00  152
 58  \w    100.00 162.00   0.50    0.20    --   94.43  83.00-178.00  124
 59  \w     99.00 156.00   0.50    0.20    --   94.43 117.00 -90.00  114
 60  \w     81.00 161.00   0.50    0.20    --   94.43 144.00 -60.00  160
 61  \w     81.00 161.00   0.50    0.20    --   94.43 144.00 -60.00  160
 62  \w    105.00 164.00   0.50    0.20    --   94.43  96.00 -60.00  118
 63  \w    105.00 164.00   0.50    0.20    --   94.43  96.00  90.00  118
 64  \w     99.00 156.00   0.50    0.20    --   94.43 117.00 150.00  114
 65  \w     15.00  43.00   0.50    0.20    --   42.38  85.00 122.81   56
;
_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      0.0310061000
_diffrn_orient_matrix_UB_12      0.0305278000
_diffrn_orient_matrix_UB_13      -0.1503440000
_diffrn_orient_matrix_UB_21      -0.0583260000
_diffrn_orient_matrix_UB_22      -0.0498905000
_diffrn_orient_matrix_UB_23      -0.0963694000
_diffrn_orient_matrix_UB_31      -0.1191010000
_diffrn_orient_matrix_UB_32      0.0323813000
_diffrn_orient_matrix_UB_33      -0.0066968000
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            42048
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.842
_diffrn_reflns_theta_min         3.836
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.558
_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    1.475
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1032
_exptl_crystal_recrystallization_method 'Solvent evaporation'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.00172(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         4163
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0379P)^2^+0.8666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3938
_reflns_number_total             4163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03087k2.cif
_cod_data_source_block           m1jan23abs
_cod_database_code               7250599
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C25 H22 F6 O4'
_cell_oxdiff_angle_alpha         90.0068(8)
_cell_oxdiff_angle_beta          94.1395(8)
_cell_oxdiff_angle_gamma         89.9984(7)
_cell_oxdiff_length_a            11.34125(9)
_cell_oxdiff_length_b            23.0434(2)
_cell_oxdiff_length_c            8.64328(10)
_cell_oxdiff_measurement_reflns_used 30411
_cell_oxdiff_volume              2252.95(4)
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.657
_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. Shared sites
{C3, C3A}
3. Restrained distances
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4
 with sigma of 0.02
 C1-C3 \\sim C1A-C3A
 with sigma of 0.04
 C2-C4 \\sim C2A-C4
 with sigma of 0.04
4. Restrained planarity
 C3A, C4, C5, C6, C7, C8, C9
 with sigma of 0.1
 C3, C4, C5, C6, C7, C8, C9
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C3A)
Uanis(C1) = Uanis(C1A)
6. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C2A)=Sof(H2A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=1-
 FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=Sof(H3B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C3A(H3AA,H3AB)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C2A(H2A)
7.c X=CH2 refined with riding coordinates:
 C1(H1A,H1B), C1A(H1AA,H1AB)
;
_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 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.772