2-(3-{(3<i>R</i>,4<i>R</i>)-4-Methyl-3-[methyl(7<i>H</i>-pyrrolo[2,3-<i>d</i>]pyrimidin-4-yl)amino]piperidin-1-yl}oxetan-3-yl)acetonitrile monohydrate
Gehringer, Matthias; Pfaffenrot, Ellen; Keck, Peter R. W. E. F.; Schollmeyer, Dieter; Laufer, Stefan A.; Acta Crystallographica Section E 70 (2014) o382–o383; doi:10.1107/S1600536814004449

data_2239217
_publ_section_title
;
 2-(3-{(3<i>R</i>,4<i>R</i>)-4-Methyl-3-[methyl(7<i>H</i>-pyrrolo[2,3-<i>d</i>]pyrimidin-4-yl)amino]piperidin-1-yl}oxetan-3-yl)acetonitrile
 monohydrate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o382
_journal_page_last               o383
_journal_paper_doi               10.1107/S1600536814004449
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C18 H24 N6 O, H2 O'
_chemical_formula_moiety         'C18 H24 N6 O, H2 O'
_chemical_formula_sum            'C18 H26 N6 O2'
_chemical_formula_weight         358.45
_chemical_name_systematic
'2-(3-{(3<i>R</i>,4<i>R</i>)-4-Methyl-3-[methyl(7<i>H</i>-pyrrolo[2,3-<i>d</i>]pyrimidin-4-yl)amino]piperidin-1-yl}oxetan-3-yl)acetonitrile monohydrate'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6088(6)
_cell_length_b                   10.1483(8)
_cell_length_c                   26.813(2)
_cell_measurement_reflns_used    6886
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.5
_cell_volume                     1798.3(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2010)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2010)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2010)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_sigmaI/netI    0.1509
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            6672
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1784
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0523P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1132
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                1716
_reflns_number_total             4184
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6965sup1.cif
_cod_data_source_block           I
_cod_database_code               2239217
_cod_database_fobs_code          2239217