Total CCl4 guest alignment in a quasiracemic clathrate closely related to Dianin’s compound
Frampton, Christopher Stephen; Gall, James H.; MacNicol, David D.; CrystEngComm  (2017) –; doi:10.1039/C7CE01275F

data_7228858
_publ_section_title
;
 Total CCl4 guest alignment in a quasiracemic clathrate closely related to
 Dianin&#x2019;s compound
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01275F
_journal_year                    2017
_chemical_formula_moiety         'C19 H22 O2'
_chemical_formula_sum            'C19 H22 O2'
_chemical_formula_weight         282.36
_chemical_name_common
;
7-Methyl Dianin's compound
;
_chemical_name_systematic
;
p-Hydroxyphenyl-2,2,4,7-tetramethylchroman
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-06-26 deposited with the CCDC.
2017-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6565(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.77030(15)
_cell_length_b                   12.02971(18)
_cell_length_c                   12.7860(2)
_cell_measurement_reflns_used    4374
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.4160
_cell_measurement_theta_min      3.5040
_cell_volume                     1502.69(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43a (Rigaku OD, 2015)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2001), <i>Mercury CSD 2.0</i> (Macrae <i>et al</i>., 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2001), <i>Mercury CSD 2.0</i> (Macrae <i>et al</i>., 2008)
;
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXD-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 5.2921
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6135
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.481
_diffrn_reflns_theta_min         5.048
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43a (Rigaku Oxford Diffraction, 2015)
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_density_diffrn    1.248
_exptl_crystal_description       Block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.207
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.0050(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0450P)^2^+0.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2866
_reflns_number_total             3058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01275f2.cif
_cod_data_source_block           b17062r
_cod_database_code               7228858
_shelx_estimated_absorpt_t_min   0.816
_shelx_estimated_absorpt_t_max   0.882
_shelxl_version_number           2014/6
_shelx_res_checksum              29996