Polymorphism through Desolvation of the Solvates of a van der Waals Host
Bhattacharya, Suman; Saha, Binoy K.; Crystal Growth & Design 13 (2013) 606–; doi:10.1021/cg301269d

data_4507199
_publ_section_title
;
 Polymorphism through Desolvation of the Solvates of a van der Waals Host
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              606
_journal_paper_doi               10.1021/cg301269d
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C33 H36 O3, C4 H8 O'
_chemical_formula_sum            'C37 H44 O4'
_chemical_formula_weight         552.72
_chemical_name_common            1H-THF(2)
_chemical_name_systematic
;
2,4,6-Triethyl-1,3,5-trisphenoxymethylbenzene , tetrahydrofuran(2)
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-30
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.697(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5713(12)
_cell_length_b                   10.3703(9)
_cell_length_c                   22.865(2)
_cell_measurement_reflns_used    4754
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.2725
_cell_measurement_theta_min      2.6700
_cell_volume                     3214.4(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   54.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2928  179.0000 -120.0000 26

  2 omega   60.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2928  179.0000   90.0000 35

  3 omega  -53.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2928    0.0000   90.0000 124

  4 omega   25.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2928   77.0000  -90.0000 63

  5 omega  -11.00   26.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2928   77.0000  150.0000 37
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0407575000
_diffrn_orient_matrix_UB_12      -0.0255270000
_diffrn_orient_matrix_UB_13      0.0168020000
_diffrn_orient_matrix_UB_21      -0.0281638000
_diffrn_orient_matrix_UB_22      0.0011351000
_diffrn_orient_matrix_UB_23      0.0253438000
_diffrn_orient_matrix_UB_31      -0.0168775000
_diffrn_orient_matrix_UB_32      -0.0634074000
_diffrn_orient_matrix_UB_33      -0.0063515000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15397
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5669
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.1671
_refine_ls_R_factor_gt           0.1165
_refine_ls_shift/su_max          0.457
_refine_ls_shift/su_mean         0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3321
_refine_ls_wR_factor_ref         0.3827
_reflns_number_gt                3234
_reflns_number_total             5669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301269d_si_001.cif
_cod_data_source_block           1H-THF(2)
_cod_original_cell_volume        3214.5(5)
_cod_database_code               4507199