On the Formation of Droperidol Solvates: Characterization of Structure and Properties
Be̅rziņš, Agris; Skarbulis, Edgards; Rekis, Toms; Actiņš, Andris; Crystal Growth & Design 14 (2014) 2654–; doi:10.1021/cg5003447

data_4510533
_publ_section_title
;
 On the Formation of Droperidol Solvates: Characterization of Structure
 and Properties
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2654
_journal_paper_doi               10.1021/cg5003447
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C22 H22 F N3 O2, 0.5(C H4 O)'
_chemical_formula_sum            'C22.5 H24 F N3 O2.5'
_chemical_formula_weight         395.45
_chemical_name_common            'droperidol methanol hemisolvate'
_chemical_name_systematic
;
1-{1-[4-(4-fluorophenyl)-4-oxobutyl]-1,2,5,6-tetrahydropyridin-4-yl]
-1,3-dihydro-2H-benzimidazol}-2-one methanol hemisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                101.397(2)
_cell_angle_beta                 93.445(3)
_cell_angle_gamma                97.022(2)
_cell_formula_units_Z            2
_cell_length_a                   6.0504(5)
_cell_length_b                   10.2207(8)
_cell_length_c                   16.1100(14)
_cell_measurement_reflns_used    2477
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.59
_cell_volume                     965.62(14)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16568
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         1.29
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_correction_T_min  0.4641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0426 before and 0.0309 after correction.
The Ratio of minimum to maximum transmission is 0.4733.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0600P)^2^+0.3300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1512
_reflns_number_gt                3333
_reflns_number_total             5392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5003447_si_007.cif
_cod_data_source_block           SMe_(droperidol_methanol_solvate)
_cod_depositor_comments
'Adding full bibliography for 4510531--4510537.cif.'
_cod_original_formula_sum        'C22.50 H24 F N3 O2.50'
_cod_database_code               4510533
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O3(0.5) H3(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
3.a Riding coordinates:
 O3(H3), C23(H23A,H23B,H23C)
;