Microbatch under-oil salt screening of organic cations: single-crystal growth of active pharmaceutical ingredients
Babor, Martin; Nievergelt, Philipp P.; Čejka, Jan; Zvoníček, Vít; Spingler, Bernhard; IUCrJ 6 (2019) 145–151; doi:10.1107/S2052252518017876

data_1550449
_publ_section_title
;
 Microbatch under-oil salt screening of organic cations: single-crystal
 growth of active pharmaceutical ingredients
;
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_page_first              145
_journal_page_last               151
_journal_paper_doi               10.1107/S2052252518017876
_journal_volume                  6
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H27 N2 O4 S, H2O4 P, 1.5(H2 O)'
_chemical_formula_sum            'C22 H32 N2 O9.5 P S'
_chemical_formula_weight         539.52
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                82.3345(7)
_cell_angle_beta                 81.4117(7)
_cell_angle_gamma                89.9824(7)
_cell_formula_units_Z            4
_cell_length_a                   8.79290(10)
_cell_length_b                   12.66450(10)
_cell_length_c                   23.7867(2)
_cell_measurement_reflns_used    109761
_cell_measurement_temperature    160
_cell_measurement_theta_max      79
_cell_measurement_theta_min      4
_cell_volume                     2595.20(4)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      160
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            264132
_diffrn_reflns_theta_full        72.109
_diffrn_reflns_theta_max         72.109
_diffrn_reflns_theta_min         3.522
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.171
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.49
_refine_diff_density_min         -0.46
_refine_ls_abs_structure_details 'Flack (1983), 9652 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.020(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1376
_refine_ls_number_reflns         19783
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.0009634
_refine_ls_shift/su_mean         0.0000379
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 1.40P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1283
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1283
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              29
_reflns_limit_l_min              -29
_reflns_number_gt                18568
_reflns_number_total             19821
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.51
_oxford_diffrn_Wilson_scale      0.38
_oxford_refine_ls_r_factor_ref   0.0519
_oxford_refine_ls_scale          1.392(4)
_oxford_reflns_number_all        19783
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            lt5016.cif
_cod_data_source_block           Diltiazemphosphatesesquihydrate
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

2019-05-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2595.21(4)
_cod_original_sg_symbol_H-M      'P 1 '
_cod_original_formula_moiety     '2(C22 H27 N2 O4 S), 2(H2O4 P), 3(H2 O)'
_cod_original_formula_sum        'C44 H64 N4 O19 P2 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1079.05
_cod_database_code               1550449