Synthesis and supramolecular properties of all-<i>cis</i>-2,4,6-trifluorocyclohexane-1,3,5-triol.
Haridas, Shyamkumar V.; von Delius, Max; Chemical communications (Cambridge, England) 60 (2024) 606–609; doi:10.1039/d3cc05510h

data_7132463
_publ_section_title
;
 Synthesis and supramolecular properties of
 all-<i>cis</i>-2,4,6-trifluorocyclohexane-1,3,5-triol.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              606
_journal_page_last               609
_journal_paper_doi               10.1039/d3cc05510h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C6 H11 F3 O4'
_chemical_formula_sum            'C6 H11 F3 O4'
_chemical_formula_weight         204.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-11-06 deposited with the CCDC.	2023-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1696(5)
_cell_length_b                   9.4705(3)
_cell_length_c                   4.82980(10)
_cell_measurement_reflns_used    2596
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      72.7800
_cell_measurement_theta_min      5.1490
_cell_volume                     785.35(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3385
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -68.00  31.00   1.00    1.00    --  -43.06  38.00 120.00   99
  2  \w   -115.00 -28.00   1.00    1.00    --  -43.06 -57.00 -30.00   87
  3  \w    -58.00  -6.00   1.00    1.00    --  -43.06 125.00-180.00   52
  4  \w     29.00  96.00   1.00    1.00    --   43.06-125.00-120.00   67
  5  \w     35.00 105.00   1.00    1.00    --  104.94 -95.00  60.00   70
  6  \w     23.00 105.00   1.00    1.00    --  104.94 -95.00 -30.00   82
  7  \w    113.00 177.00   1.00    1.00    --  104.94  77.00 120.00   64
  8  \w     78.00 136.00   1.00    1.00    --  104.94  30.00  60.00   58
  9  \w     88.00 114.00   1.00    1.00    --  104.94 -30.00  60.00   26
 10  \w     42.00 110.00   1.00    1.00    --  104.94-125.00-120.00   68
 11  \w     44.00  77.00   1.00    1.00    --  104.94 -30.00  60.00   33
 12  \w     63.00 135.00   1.00    1.00    --  104.94 -66.00  40.00   72
 13  \w    102.00 165.00   1.00    1.00    --  104.94 125.00  30.00   63
 14  \w    121.00 172.00   1.00    1.00    --  104.94  30.00   0.00   51
 15  \w     83.00 108.00   1.00    1.00    --  104.94-104.00-107.18   25
 16  \w     86.00 161.00   1.00    1.00    --  104.94  45.00  90.00   75
 17  \w     26.00  62.00   1.00    1.00    --  104.94-104.00-107.18   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0212287000
_diffrn_orient_matrix_UB_12      0.0663548000
_diffrn_orient_matrix_UB_13      -0.2813539000
_diffrn_orient_matrix_UB_21      0.0650017000
_diffrn_orient_matrix_UB_22      -0.0863854000
_diffrn_orient_matrix_UB_23      -0.1402292000
_diffrn_orient_matrix_UB_31      -0.0581069000
_diffrn_orient_matrix_UB_32      -0.1207561000
_diffrn_orient_matrix_UB_33      -0.0543410000
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4748
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.044
_diffrn_reflns_theta_min         5.152
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       needle
_exptl_crystal_F_000             424
_exptl_crystal_preparation       'Recrystallized from Acetone'
_exptl_crystal_recrystallization_method 'Recrystallized from Acetone'
_exptl_crystal_size_max          0.519
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0482P)^2^+0.5166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                763
_reflns_number_total             821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05510h2.cif
_cod_data_source_block           svh21049
_cod_depositor_comments
'Adding full bibliography for 7132462--7132465.cif.'
_cod_database_code               7132463
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C6 H9 O3 F3'
_chemical_oxdiff_usercomment     SVH-120-MeOH/Acetone
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.480
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: H00B(0.5) H004(0.5)
2.a Free rotating group:
 O003(H00A,H00B)
2.b Ternary CH refined with riding coordinates:
 C006(H006), C007(H007), C008(H008), C009(H009)
2.c Idealised tetrahedral OH refined as rotating group:
 O004(H004), O005(H005)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.950
_oxdiff_exptl_absorpt_empirical_full_min 0.463