1-{3-[(7-Fluoro-9<i>H</i>-pyrimido[4,5-<i>b</i>]indol-4-yl)(methyl)amino]piperidin-1-yl}propan-1-one
Andreev, Stanislav; Schollmeyer, Dieter; Koch, Pierre; IUCrData 6 (2021) x210159–; doi:10.1107/S2414314621001590

data_1560706
_publ_section_title
;
 1-{3-[(7-Fluoro-9<i>H</i>-pyrimido[4,5-<i>b</i>]indol-4-yl)(methyl)amino]piperidin-1-yl}propan-1-one
;
_journal_coeditor_code           BT4108
_journal_issue                   2
_journal_name_full               IUCrData
_journal_page_first              x210159
_journal_paper_doi               10.1107/S2414314621001590
_journal_volume                  6
_journal_year                    2021
_chemical_formula_iupac          'C19 H22 F N5 O'
_chemical_formula_moiety         'C19 H22 F N5 O'
_chemical_formula_sum            'C19 H22 F N5 O'
_chemical_formula_weight         355.41
_chemical_name_systematic
1-{3-[(7-Fluoro-9<i>H</i>-pyrimido[4,5-<i>b</i>]indol-4-yl)(methyl)amino]piperidin-1-yl}propan-1-one
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.6982(3)
_cell_length_b                   19.8473(8)
_cell_length_c                   16.7642(6)
_cell_measurement_reflns_used    7975
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.38
_cell_volume                     3559.5(2)
_computing_cell_refinement
;
X-Area <i>Recipe</i> (Stoe & Cie, 2019)
;
_computing_data_collection
;
X-Area <i>WinXpose</i> (Stoe & Cie, 2019)
;
_computing_data_reduction
;
X-Area <i>Integrate</i> (Stoe & Cie, 2019)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.894
_diffrn_reflns_theta_min         2.385
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.410
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+2.3561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                2840
_reflns_number_total             4202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4108sup1.cif
_cod_data_source_block           I
_cod_database_code               1560706
_cod_database_fobs_code          1560706
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.993
_shelx_hkl_checksum              19171
_shelx_res_checksum              93963