Dianin's compound trichloroacetonitrile clathrate
Tia Jacobs; Gareth O. Lloyd; Martin W. Bredenkamp; Acta Crystallographica Section E 62 (2006) o4400–o4402; doi:10.1107/S1600536806035884

data_2210651
_publ_section_title
;
 Dianin's compound trichloroacetonitrile clathrate
;
_journal_coeditor_code           HG2106
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4400
_journal_page_last               o4402
_journal_paper_doi               10.1107/S1600536806035884
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '6C18 H20 O2 , C2 Cl3 N'
_chemical_formula_moiety         '6C18 H20 O2 , C2 Cl3 N'
_chemical_formula_sum            'C110 H120 Cl3 N O12'
_chemical_formula_weight         1754.42
_chemical_name_common
;
Dianin's compound trichloroacetonitrile clathrate
;
_chemical_name_systematic
;
4-(2,2,4-trimethylchroman-4-yl)phenol--trichloroacetonitrile (6/1)
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   26.8141(13)
_cell_length_b                   26.8141(13)
_cell_length_c                   10.8765(11)
_cell_measurement_reflns_used    4788
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.142
_cell_measurement_theta_min      2.566
_cell_volume                     6772.5(8)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'X-SEED (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_publication_material  X-SEED
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            14334
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2802
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.452
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3553
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.087P)^2^+2.3737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                2904
_reflns_number_total             3553
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2106.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C110 H120 Cl3 N1 O12'
_cod_database_code               2210651
_cod_database_fobs_code          2210651