A high throughput screening method for the nano-crystallization of salts of organic cations.
Nievergelt, Philipp P.; Babor, Martin; Čejka, Jan; Spingler, Bernhard; Chemical science 9 (2018) 3716–3722; doi:10.1039/c8sc00783g

data_1549045
_publ_section_title
;
 A high throughput screening method for the nano-crystallization of salts
 of organic cations.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              3716
_journal_page_last               3722
_journal_paper_doi               10.1039/c8sc00783g
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         '2(C19 H23 Cl N5 O), C2 O4, 10(H2 O)'
_chemical_formula_sum            'C40 H66 Cl2 N10 O16'
_chemical_formula_weight         1013.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-07 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.293(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1489(4)
_cell_length_b                   13.2904(4)
_cell_length_c                   24.5940(8)
_cell_measurement_reflns_used    10679
_cell_measurement_temperature    159.95(10)
_cell_measurement_theta_max      76.4470
_cell_measurement_theta_min      3.2740
_cell_volume                     4911.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      159.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -116.00 -18.00   1.00   15.00    --  -41.94 -37.00 -60.00   98
  2  \w     18.00 116.00   1.00   15.00    --   41.94  37.00 150.00   98
  3  \w    -33.00  66.00   1.00   15.00    --   41.94 -37.00 -30.00   99
  4  \w    -30.00  70.00   1.00   15.00    --   41.94 -57.00-150.00  100
  5  \w     86.00 178.00   1.00   60.00    --  112.00  45.00 -60.00   92
  6  \w     84.00 178.00   1.00   60.00    --  112.00  30.00  30.00   94
  7  \w     39.00 138.00   1.00   60.00    --  112.00 -45.00 -60.00   99
  8  \w     86.00 178.00   1.00   60.00    --  112.00  45.00 -90.00   92
  9  \w     86.00 178.00   1.00   60.00    --  112.00  45.00-180.00   92
 10  \w     84.00 178.00   1.00   60.00    --  112.00  30.00  60.00   94
 11  \w     40.00 141.00   1.00   60.00    --  112.00 -60.00 -59.62  101
 12  \w     40.00 141.00   1.00   60.00    --  112.00 -60.00 -89.82  101
 13  \w     36.00 140.00   1.00   60.00    --  112.00 -30.00  90.00  104
 14  \w     86.00 178.00   1.00   60.00    --  112.00  45.00 -30.00   92
 15  \w     14.00  46.00   1.00   15.00    --   41.94  58.00-119.55   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0135329000
_diffrn_orient_matrix_UB_12      -0.0560910000
_diffrn_orient_matrix_UB_13      0.0531340000
_diffrn_orient_matrix_UB_21      -0.1007169000
_diffrn_orient_matrix_UB_22      -0.0063449000
_diffrn_orient_matrix_UB_23      -0.0191201000
_diffrn_orient_matrix_UB_31      0.0138160000
_diffrn_orient_matrix_UB_32      -0.1013044000
_diffrn_orient_matrix_UB_33      -0.0281604000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20149
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.973
_diffrn_reflns_theta_min         3.624
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (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_colour_primary    colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       needle
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5113
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+3.9562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4562
_reflns_number_total             5113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00783g2.cif
_cod_data_source_block           pn181016o_10453_b9_d3_traz_ox_4
_cod_depositor_comments
'Adding full bibliography for 1549042--1549063.cif.'
_cod_database_code               1549045
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C40 H60 N10 O16 Cl2'
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.782
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O31-H31A = O31-H31B = O32-H32A = O34-H34B
 0.83 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,
 H16B), C18(H18A,H18B), C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C21(H21), C23(H23), C24(H24), C25(H25)
;
_shelx_res_checksum              14858
_shelx_hkl_checksum              77410
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.636
_oxdiff_exptl_absorpt_empirical_full_min 0.707