Crystal structure of 2,6-bis(3-hydroxy-3-methylbut-1-yn-1-yl)pyridine monohydrate
Koizumi, Take-aki; Takata, Toshikazu; Acta Crystallographica Section E 76 (2020) 1737–1740; doi:10.1107/S2056989020013304

data_2243619
_publ_section_title
;
 Crystal structure of 2,6-bis(3-hydroxy-3-methylbut-1-yn-1-yl)pyridine
 monohydrate
;
_journal_coeditor_code           IS5553
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1737
_journal_page_last               1740
_journal_paper_doi               10.1107/S2056989020013304
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C15 H17 N O2, H2 O'
_chemical_formula_moiety         'C15 H17 N O2, H2 O'
_chemical_formula_sum            'C15 H19 N O3'
_chemical_formula_weight         261.31
_chemical_name_common
;
2,6-Bis(3-hydroxy-3-methylbut-1-yn-1-yl)pyridine monohydrate
;
_chemical_name_systematic
;
4-[6-(3-Hydroxy-3-methylbut-1-yn-1-yl)pyridin-2-yl]-2-methylbut-3-yn-2-ol
monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   31.9834(14)
_cell_length_b                   27.7358(13)
_cell_length_c                   6.6610(4)
_cell_measurement_reflns_used    4276
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      74.9060
_cell_measurement_theta_min      4.1790
_cell_volume                     5908.9(5)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>Olex2.refine</i> (Bourhis <i>et al.</i>,  2015)
;
_computing_structure_solution
;
<i>Olex2.solve</i> (Bourhis <i>et al.</i>,  2015)
;
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0145
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4676
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.961
_diffrn_reflns_theta_min         4.220
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.195
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 495 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.02(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2071
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0555P)^2^+3.7832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                2045
_reflns_number_total             2071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5553sup1.cif
_cod_data_source_block           I
_cod_database_code               2243619
_cod_database_fobs_code          2243619
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.937
_shelx_hkl_checksum              26960
_shelx_res_checksum              31723