Functionalised polyhedral oligomeric silsesquioxane with encapsulated fluoride - first observation of fluxional SiF interactions in POSS.
Laird, Mathilde; Totée, Cédric; Gaveau, Philippe; Silly, Gilles; Van der Lee, Arie; Carcel, Carole; Unno, Masafumi; Bartlett, John R.; Wong Chi Man, Michel; Dalton transactions (Cambridge, England : 2003) 50 (2021) 81–89; doi:10.1039/d0dt03057k

data_7706340
_publ_section_title
;
 Functionalised polyhedral oligomeric silsesquioxane with encapsulated
 fluoride - first observation of fluxional SiF interactions in POSS.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              81
_journal_page_last               89
_journal_paper_doi               10.1039/d0dt03057k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '3(C64 H56 O12 Si8), 2(C16 H36 N), 3(F)'
_chemical_formula_sum            'C224 H240 F3 N2 O36 Si24'
_chemical_formula_weight         4267.35
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_update_record
;
2020-07-23 deposited with the CCDC.	2020-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                80.895(5)
_cell_angle_beta                 81.259(5)
_cell_angle_gamma                81.193(4)
_cell_formula_units_Z            1
_cell_length_a                   13.6092(7)
_cell_length_b                   13.6117(7)
_cell_length_c                   39.217(2)
_cell_measurement_reflns_used    6318
_cell_measurement_temperature    175
_cell_measurement_theta_max      20.6210
_cell_measurement_theta_min      2.0310
_cell_volume                     7027.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0143
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -14.00  27.00   1.00  195.00    --   -5.54-100.00  30.00   41
  2  \w    -17.00  47.00   1.00  195.00    --    6.24-100.00 -30.00   64
  3  \w    -12.00  75.00   1.00  195.00    --    6.24  57.00-150.00   87
  4  \w    -21.00  11.00   1.00  195.00    --    6.24-100.00-150.00   32
  5  \w    -32.00  79.00   1.00  195.00    --    6.24  19.00 150.00  111
;
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0099898000
_diffrn_orient_matrix_UB_12      -0.0510754000
_diffrn_orient_matrix_UB_13      -0.0027130000
_diffrn_orient_matrix_UB_21      0.0315975000
_diffrn_orient_matrix_UB_22      -0.0102303000
_diffrn_orient_matrix_UB_23      0.0132773000
_diffrn_orient_matrix_UB_31      -0.0416277000
_diffrn_orient_matrix_UB_32      -0.0110215000
_diffrn_orient_matrix_UB_33      0.0125269000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_unetI/netI     0.1539
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14685
_diffrn_reflns_theta_full        20.831
_diffrn_reflns_theta_max         20.831
_diffrn_reflns_theta_min         1.736
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2249
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1303
_refine_ls_number_reflns         10540
_refine_ls_number_restraints     512
_refine_ls_R_factor_all          0.1525
_refine_ls_R_factor_gt           0.1284
_refine_ls_shift/su_max          0.0014883
_refine_ls_shift/su_mean         0.0000195
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are:
 17.1 6.23 10.8 3.99 -0.739
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1641
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1402
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                10540
_reflns_number_total             14685
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.33
_oxford_diffrn_Wilson_scale      0.82
_oxford_refine_ls_r_factor_ref   0.1284
_oxford_refine_ls_scale          1.687(5)
_oxford_reflns_number_all        14685
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            d0dt03057k2.cif
_cod_data_source_block           1
_cod_original_cell_volume        7027.7(4)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7706340
_cell_oxdiff_length_a            13.6092(7)
_cell_oxdiff_length_b            13.6117(7)
_cell_oxdiff_length_c            39.217(2)
_cell_oxdiff_angle_alpha         80.895(5)
_cell_oxdiff_angle_beta          81.259(5)
_cell_oxdiff_angle_gamma         81.193(4)
_cell_oxdiff_volume              7027.7(6)
_oxdiff_exptl_absorpt_empirical_full_min 0.823
_oxdiff_exptl_absorpt_empirical_full_max 1.135
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_montpellier_reflns_maxres       1.19
_montpellier_reflns_completeness_maxres 99.85
_montpellier_reflns_redundancy_maxres 2.92
_publcif_funding_html
;
;