Improved Synthesis and Crystal Structure of Dalcetrapib
Laus, Gerhard; Kahlenberg, Volker; Richter, Frank; Nerdinger, Sven; Schottenberger, Herwig; Crystals 2 (2012) 1455–1459; doi:10.3390/cryst2041455

data_1508401
_publ_section_title
;
 Improved Synthesis and Crystal Structure of Dalcetrapib
;
_journal_issue                   4
_journal_name_full               Crystals
_journal_page_first              1455
_journal_page_last               1459
_journal_paper_doi               10.3390/cryst2041455
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C23 H35 N O2 S'
_chemical_formula_sum            'C23 H35 N O2 S'
_chemical_formula_weight         389.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-08-03T12:43:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.003(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7572(3)
_cell_length_b                   9.7154(3)
_cell_length_c                   20.5873(6)
_cell_measurement_reflns_used    4977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.1428
_cell_measurement_theta_min      4.1117
_cell_volume                     2151.59(11)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla et al., 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3822
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1095038409
_diffrn_orient_matrix_UB_12      0.0796372053
_diffrn_orient_matrix_UB_13      0.0304308365
_diffrn_orient_matrix_UB_21      -0.0468975288
_diffrn_orient_matrix_UB_22      0.1334297107
_diffrn_orient_matrix_UB_23      -0.0317639351
_diffrn_orient_matrix_UB_31      -0.079728163
_diffrn_orient_matrix_UB_32      0.0311512983
_diffrn_orient_matrix_UB_33      0.0607239756
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13476
_diffrn_reflns_theta_full        67.18
_diffrn_reflns_theta_max         67.18
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.79729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3624
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                2668
_reflns_number_total             3624
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file
C23H35NO2S_P21_c_crystals-02-01455-s001_DC146.cif
_cod_data_source_block           gl398_1_chateigner_1508401
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_database_code               1508401