Thermally stable polyfluorinated monoalkoxysilanetriols and dialkoxydisiloxanetetrols
Feige, Felix; Kögel, Julius F.; Lork, Enno; Beckmann, Jens; Dalton Transactions  (2021) –; doi:10.1039/D1DT03389A

data_7709005
_publ_section_title
;
 Thermally stable polyfluorinated monoalkoxysilanetriols and
 dialkoxydisiloxanetetrols
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03389A
_journal_year                    2021
_chemical_formula_moiety         'C50 H22 F36 O7 Si2, C4 H10 O'
_chemical_formula_sum            'C54 H32 F36 O8 Si2'
_chemical_formula_weight         1548.97
_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
_audit_creation_date             2020-12-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-05 deposited with the CCDC.	2021-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.562(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8065(7)
_cell_length_b                   25.8702(10)
_cell_length_c                   18.0791(8)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.20
_cell_volume                     6189.5(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            164878
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.288
_diffrn_reflns_theta_min         2.186
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7167
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0727 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.9601.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         1.960
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         15340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0753P)^2^+10.9707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11621
_reflns_number_total             15340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03389a2.cif
_cod_data_source_block           feigef201110_0m
_cod_database_code               7709005
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Others
 Fixed Sof: F25(0.5) F28(0.5) F63(0.6) F66(0.5) F67(0.25) F70(0.6) F02P(0.5)
 F02R(0.5) F1(0.5) F0AA(0.5) F65(0.5) F68(0.6) F71(0.3) F64(0.4) F27(0.5)
 F24(0.5) F69(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C15(H15), C45(H45), C11(H11), C21(H21), C51(H51), C65(H65),
 C53(H53), C35(H35), C31(H31), C43(H43), C25(H25), C13(H13), C55(H55), C23(H23),
  C33(H33), C63(H63), C61(H61)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C4(H4A,H4B,H4C)
3.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O7(H7), O6(H6), O3(H3)
;
_shelx_res_checksum              51061
_shelx_hkl_checksum              19646
_olex2_submission_special_instructions 'No special instructions were received'