Combined crystal structure prediction and high-pressure crystallization in rational pharmaceutical polymorph screening
M. A. Neumann; J. van de Streek; F. P. A. Fabbiani; P. Hidber; O. Grassmann; Nature Communications 6 (2015) 7793–; doi:10.1038/ncomms8793

data_1548159
_publ_section_title
;
 Combined crystal structure prediction and high-pressure crystallization
 in rational pharmaceutical polymorph screening
;
_journal_name_full               'Nature Communications'
_journal_page_first              7793
_journal_paper_doi               10.1038/ncomms8793
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C23 H35 N O2 S'
_chemical_formula_sum            'C23 H35 N O2 S'
_chemical_formula_weight         389.58
_chemical_name_common            Dalcetrapib
_chemical_name_systematic
;
S-[2-({[1-(2-ethylbutyl)cyclohexyl]carbonyl}amino)phenyl] 2-methylpropanethioate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     'known structure'
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 88.7400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2235(3)
_cell_length_b                   9.8526(2)
_cell_length_c                   20.7922(5)
_cell_measurement_reflns_used    6329
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.99
_cell_measurement_theta_min      2.64
_cell_volume                     2298.66(9)
_computing_cell_refinement       'APEX2 v2012.4-0'
_computing_data_collection       'APEX2 v2012.4-0'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    Sir92
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17030
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.718
_diffrn_reflns_theta_min         1.815
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.8619
_exptl_absorpt_correction_T_min  0.7919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 2012<i>a</i>)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.0057(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3894
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.9076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1564
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3112
_reflns_number_total             3894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms8793-s3.cif
_cod_data_source_block           FormA_RT
_cod_database_code               1548159