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

data_7709003
_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         'C38 H4 F30 O7 Si2'
_chemical_formula_sum            'C38 H4 F30 O7 Si2'
_chemical_formula_weight         1198.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-10
_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                108.150(4)
_cell_angle_beta                 104.185(4)
_cell_angle_gamma                100.559(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0814(13)
_cell_length_b                   13.9764(15)
_cell_length_c                   14.1905(17)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.16
_cell_volume                     1942.7(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'XM  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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  0.0719
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44012
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.462
_diffrn_reflns_theta_min         1.976
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5481
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0978 before and 0.0801 after correction.
The Ratio of minimum to maximum transmission is 0.7350.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .2
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         9698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0621
_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^)+(0.1122P)^2^+1.2350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7278
_reflns_number_total             9698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03389a2.cif
_cod_data_source_block           feigef201030_0m
_cod_database_code               7709003
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2.a Idealised tetrahedral OH refined as rotating group:
 O6(H6), O7(H7), O2(H2), O3(H3)
;
_shelx_res_checksum              22994
_shelx_hkl_checksum              71858
_olex2_submission_special_instructions 'No special instructions were received'