A new olanzapine cocrystal obtained from volatile deep eutectic solvents and determined by 3D electron diffraction
Andrusenko, Iryna; Potticary, Jason; Hall, Simon R.; Gemmi, Mauro; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620012779

data_2108734
_publ_section_title
;
 A new olanzapine cocrystal obtained from volatile deep eutectic solvents
 and determined by 3D electron diffraction
;
_journal_coeditor_code           JE5035SUP1
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620012779
_journal_volume                  76
_journal_year                    2020
_chemical_formula_sum            'C23 H26 N4 O S'
_chemical_formula_weight         406.55
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2020-06-10T11:02
_audit_creation_method           'created in GSAS-II'
_audit_update_record
'2020-06-10T11:02  Initial software-generated CIF'
_cell_angle_alpha                96.686(4)
_cell_angle_beta                 95.2878(27)
_cell_angle_gamma                104.474(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4051(9)
_cell_length_b                   10.4236(11)
_cell_length_c                   11.9619(8)
_cell_volume                     1118.74(18)
_computing_structure_refinement
'GSAS-II (Toby & Von Dreele, J. Appl. Cryst. 46, 544-549, 2013)'
_diffrn_ambient_pressure         100
_diffrn_ambient_temperature      300
_diffrn_radiation_polarisn_ratio 0.5000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           K\a~1,2~
_exptl_crystal_density_diffrn    1.2069
_pd_block_id
;
2020-06-10T11:02|OL-PH_03_5-50_ip_RBola+pheH_str_XYW_str+harm_OH|IIT|stoe
;
_pd_calc_method                  'Rietveld Refinement'
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.01500
_pd_meas_2theta_range_max        59.99500
_pd_meas_2theta_range_min        4.00000
_pd_meas_number_of_points        3734
_pd_phase_name                   OL-PH
_pd_proc_info_datetime           2020-06-10T11:02
_pd_proc_info_excluded_regions   ' ?'
_pd_proc_ls_background_function
;
Background function: "chebyschev" function with 25 terms:
    7528.037, -14417.256, 50354.276, -121521.867, -509603.960, 
    2.463542149e6, 1.375028072e6, -1.5190601545e7, 1.352714535e6, 
    4.9241608545e7, -1.5061510216e7, -9.5148349902e7, 3.4809089448e7, 
    1.13563957926e8, -3.9085584723e7, -8.2281996819e7, 2.2129096132e7, 
    3.3235336189e7, -5.056568913e6, -5.752643212e6, -3104.739, 
    679.624, -3054.502, 2044.371, 973.880, 
;
_pd_proc_ls_pref_orient_corr
;
Simple spherical harmonic correction Order = 10
    Coefficients:  0:0:C(2,-2) = 0.059(23); 0:0:C(2,-1) = 0.128(27); 
    0:0:C(2,0) = 0.09(4); 0:0:C(2,1) = -0.182(25); 0:0:C(2,2) = 0.053(28); 
    0:0:C(4,-4) = 0.25(5); 0:0:C(4,-3) = 0.03(5); 0:0:C(4,-2) = 0.34(5); 
    0:0:C(4,-1) = 0.22(5); 0:0:C(4,0) = 0.06(7); 0:0:C(4,1) = -0.26(6); 
    0:0:C(4,2) = 0.26(5); 0:0:C(4,3) = -0.16(5); 0:0:C(4,4) = 0.71(5); 
    0:0:C(6,-6) = -0.35(10); 0:0:C(6,-5) = 1.54(8); 0:0:C(6,-4) = -0.88(9); 
    0:0:C(6,-3) = 0.08(8); 0:0:C(6,-2) = -0.08(9); 0:0:C(6,-1) = -1.11(10); 
    0:0:C(6,0) = 0.65(12); 0:0:C(6,1) = 0.26(8); 0:0:C(6,2) = 0.54(8); 
    0:0:C(6,3) = -0.15(10); 0:0:C(6,4) = 0.63(7); 0:0:C(6,5) = -0.25(9); 
    0:0:C(6,6) = 0.24(9); 0:0:C(8,-8) = 0.04(17); 0:0:C(8,-7) = -0.36(16); 
    0:0:C(8,-6) = 0.12(12); 0:0:C(8,-5) = 0.30(15); 0:0:C(8,-4) = -0.45(15); 
    0:0:C(8,-3) = -0.85(17); 0:0:C(8,-2) = -0.11(19); 0:0:C(8,-1) = 0.13(13); 
    0:0:C(8,0) = -2.52(19); 0:0:C(8,1) = -1.49(22); 0:0:C(8,2) = 0.61(17); 
    0:0:C(8,3) = -0.16(14); 0:0:C(8,4) = 0.70(14); 0:0:C(8,5) = 1.39(11); 
    0:0:C(8,6) = -0.74(12); 0:0:C(8,7) = 1.62(17); 0:0:C(8,8) = -2.66(18); 
    0:0:C(10,-10) = 0.32(15); 0:0:C(10,-9) = 0.74(17); 0:0:C(10,-8) = 1.15(18); 
    0:0:C(10,-7) = 0.61(15); 0:0:C(10,-6) = -1.50(16); 0:0:C(10,-5) = 0.27(18); 
    0:0:C(10,-4) = -0.26(16); 0:0:C(10,-3) = -0.53(17); 0:0:C(10,-2) = -0.17(17); 
    0:0:C(10,-1) = -0.50(18); 0:0:C(10,0) = 1.63(13); 0:0:C(10,1) = 2.68(19); 
    0:0:C(10,2) = 0.95(13); 0:0:C(10,3) = 0.87(17); 0:0:C(10,4) = -0.10(17); 
    0:0:C(10,5) = 0.88(19); 0:0:C(10,6) = -1.91(13); 0:0:C(10,7) = -0.81(13); 
    0:0:C(10,8) = 0.55(17); 0:0:C(10,9) = 0.25(16); 0:0:C(10,10) = -0.47(16); 
;
_pd_proc_ls_profile_function
;
Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L:
  peak variance(Gauss) = Utan(Th)^2^+Vtan(Th)+W:
  peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L
  U, V, W in (centideg)^2^, X & Y in centideg
    -325.033, 214.997, -21.794, -1.295, -10.307, 0.049, 
  Crystallite size in microns with "isotropic" model:
  parameters: Size, G/L mix
    0.197(4), 1.000, 
  Microstrain, "isotropic" model (10^6^ * delta Q/Q)
    parameters: Mustrain, G/L mix
    7.23(12)e3, 1.000, 

;
_pd_proc_ls_prof_R_factor        0.02273
_pd_proc_ls_prof_wR_expected     0.01043
_pd_proc_ls_prof_wR_factor       0.03019
_pd_spec_mounting                ' ?'
_refine_ls_goodness_of_fit_all   2.931
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_R_Fsqd_factor         0.03512
_refine_ls_shift/su_max          0.5784
_refine_ls_wR_factor_obs         0.03019
_reflns_d_resolution_high        1.831
_reflns_d_resolution_low         11.786
_reflns_limit_h_max              5
_reflns_limit_h_min              0
_reflns_limit_k_max              5
_reflns_limit_k_min              -5
_reflns_limit_l_max              6
_reflns_limit_l_min              -6
_reflns_number_total             386
_cod_data_source_file            je5035sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        1118.75(5)
_cod_database_code               2108734
_refine_ls_r_f_factor            0.03849
_gsas_proc_ls_prof_r_b_factor    0.02245
_gsas_proc_ls_prof_wr_b_factor   0.02760