Structural Characterization and Rationalization of Formation, Stability, and Transformations of Benperidol Solvates
Be̅rziņš, Agris; Skarbulis, Edgars; Actiņš, Andris; Crystal Growth & Design 15 (2015) 2337–; doi:10.1021/acs.cgd.5b00138

data_4513139
_publ_section_title
;
 Structural Characterization and Rationalization of Formation, Stability,
 and Transformations of Benperidol Solvates
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2337
_journal_paper_doi               10.1021/acs.cgd.5b00138
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C22 H24 F N3 O2, 2(H2 O)'
_chemical_formula_sum            'C22 H28 F N3 O4'
_chemical_formula_weight         417.481
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 91.7206(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0595(3)
_cell_length_b                   9.3896(2)
_cell_length_c                   20.4456(6)
_cell_measurement_reflns_used    11568
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      0.9
_cell_volume                     2122.20(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_publication_material  'maXus(Mackay et al., 1999)'
_computing_structure_refinement  'maXus(Mackay et al., 1999)'
_computing_structure_solution
'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01196
_diffrn_orient_matrix_UB_12      0.05793
_diffrn_orient_matrix_UB_13      -0.06844
_diffrn_orient_matrix_UB_21      0.01005
_diffrn_orient_matrix_UB_22      -0.08179
_diffrn_orient_matrix_UB_23      -0.06747
_diffrn_orient_matrix_UB_31      -0.04807
_diffrn_orient_matrix_UB_32      0.00154
_diffrn_orient_matrix_UB_33      -0.00903
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8786
_diffrn_reflns_theta_full        29.5
_diffrn_reflns_theta_max         29.5
_diffrn_reflns_theta_min         1.8
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.63
_refine_diff_density_rms         0.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.360
_refine_ls_goodness_of_fit_gt    1.243
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3734
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.088
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details     ' w = 1 / ( s^2^(Fo^2^) + 0.10000 * Fo^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.297
_refine_ls_wR_factor_gt          0.196
_refine_ls_wR_factor_ref         0.196
_reflns_d_resolution_high        0.61
_reflns_d_resolution_low         2.26
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                3738
_reflns_number_total             5709
_reflns_threshold_expression     'I> 3.00 sigma(I)'
_cod_data_source_file            cg5b00138_si_002.cif
_cod_data_source_block           Benperidol_D
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/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 3271 2015-04-21 07:52:19Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom, diff' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n        '
_cod_original_formula_sum        'C22 H28 F N3 O4 '
_cod_database_code               4513139