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

data_7709006
_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         'C19 H3 F15 O4 Si, 0.5(C4 H10 O), 0.5(C6 H6)'
_chemical_formula_sum            'C24 H11 F15 O4.5 Si'
_chemical_formula_weight         684.41
_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   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                90
_cell_angle_beta                 101.2010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.0975(4)
_cell_length_b                   26.7831(9)
_cell_length_c                   15.9648(5)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.05
_cell_measurement_theta_min      2.47
_cell_volume                     5074.2(3)
_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 0.999
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            285954
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.085
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7134
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1145 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.9557.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .1
_refine_diff_density_max         1.594
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         12569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0605P)^2^+8.2215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10810
_reflns_number_total             12569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03389a2.cif
_cod_data_source_block           feigef201012_0m
_cod_depositor_comments
;

2025-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H22 F30 O9 Si2'
_cod_original_formula_weight         1368.83
_cod_original_formula_moiety         '2(C19 H3 F15 O4 Si), C4 H10 O, C6 H6'
_cod_original_formula_units_Z            4
_cod_database_code               7709006
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C73(H73), C71(H71), C70(H70), C72(H72), C75(H75), C74(H74)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
2.d Idealised tetrahedral OH refined as rotating group:
 O7(H7), O8(H8), O6(H6), O3(H3), O4(H4), O2(H2)
;
_shelx_res_checksum              80194
_shelx_hkl_checksum              29661
_olex2_submission_special_instructions 'No special instructions were received'