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_4507193
_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 O2'
_chemical_formula_sum            'C37 H44 O5'
_chemical_formula_weight         568.72
_chemical_name_common            1H-EAC
_chemical_name_systematic
;
2,4,6-Triethyl-1,3,5-trisphenoxymethylbenzene , ethyl acetate solvate
;
_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             2012-07-19
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.04 svn.r2321, GUI svn.r4222)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.063(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.468(2)
_cell_length_b                   9.124(10)
_cell_length_c                   20.1596(18)
_cell_measurement_reflns_used    5828
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.1510
_cell_measurement_theta_min      2.8195
_cell_volume                     3280(4)
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -58.00  -32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6522  179.0000 -180.0000 26

  2 omega   45.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4491  179.0000  -30.0000 49

  3 omega   -6.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4491   77.0000   90.0000 96

  4 omega  -52.00   21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4491  -37.0000  -30.0000 73

  5 omega   -6.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4491   37.0000  -30.0000 45
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0347917000
_diffrn_orient_matrix_UB_12      0.0120684000
_diffrn_orient_matrix_UB_13      0.0078131000
_diffrn_orient_matrix_UB_21      0.0190882000
_diffrn_orient_matrix_UB_22      0.0285958000
_diffrn_orient_matrix_UB_23      0.0325297000
_diffrn_orient_matrix_UB_31      -0.0017801000
_diffrn_orient_matrix_UB_32      0.0711560000
_diffrn_orient_matrix_UB_33      -0.0143781000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15606
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.972
_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            colourless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.0084(9)
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         5770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.2722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1740
_reflns_number_gt                2991
_reflns_number_total             5770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301269d_si_001.cif
_cod_data_source_block           1H-EAC
_cod_database_code               4507193