9α-Hydroxy-4,8-dimethyl-3'-phenyl-3,14-dioxatricyclo[9.3.0.0^2,4^]tetradec-7-en-13-one-12-spiro-5'-isoxazole monohydrate
Outahar, Fatima; Hannioui, Abdellah; Rakib, El Mostapha; Akssira, Mohamed; Saadi, Mohamed; El Ammari, Lahcen; IUCrData 4 (2019) x191408–; doi:10.1107/S2414314619014081

data_1552551
_publ_section_title
;
 9\a-Hydroxy-4,8-dimethyl-3'-phenyl-3,14-dioxatricyclo[9.3.0.0^2,4^]tetradec-7-en-13-one-12-spiro-5'-isoxazole
 monohydrate
;
_journal_coeditor_code           HB4321
_journal_issue                   10
_journal_name_full               IUCrData
_journal_page_first              x191408
_journal_paper_doi               10.1107/S2414314619014081
_journal_volume                  4
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_iupac          'C22 H25 N O5, H2 O'
_chemical_formula_moiety         'C22 H25 N O5, H2 O'
_chemical_formula_sum            'C22 H27 N O6'
_chemical_formula_weight         401.44
_chemical_name_systematic
'9\a-Hydroxy-4,8-dimethyl-3'-phenyl-3,14-dioxatricyclo[9.3.0.0^2,4^]tetradec-7-en-13-one-12-spiro-5'-isoxazole monohydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8947(4)
_cell_length_b                   10.6554(4)
_cell_length_c                   19.0286(8)
_cell_measurement_reflns_used    5184
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.696
_cell_measurement_theta_min      2.320
_cell_volume                     2006.22(14)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
WinGX and ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
Mercury (Macrae <i>et al.</i>, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXTL2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'PHOTON100 CMOS area-detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE Super DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS mirror optics'
_diffrn_radiation_source         'INCOATEC I\mS micro-focus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60442
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.696
_diffrn_reflns_theta_min         2.320
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       Block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.237
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1582 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_coef       0.020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5184
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0542P)^2^+0.2739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                4262
_reflns_number_total             5184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb4321sup1.cif
_cod_data_source_block           I
_cod_database_code               1552551
_cod_database_fobs_code          1552551
_shelx_hkl_checksum              10479
_shelx_res_checksum              63410