Ethyl 10α-hydroxy-4,9-dimethyl-14-oxo-3,8,15-trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]pentadecane-13-spiro-5'-pyrazole-3'-carboxylate
Outahar, Fatima; Moumou, Mohamed; Rakib, El Mostapha; Hannioui, Abdellah; Saadi, Mohamed; El Ammari, Lahcen; IUCrData 5 (2020) x200945–; doi:10.1107/S2414314620009451

data_1558658
_publ_section_title
;
 Ethyl
 10\a-hydroxy-4,9-dimethyl-14-oxo-3,8,15-trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]pentadecane-13-spiro-5'-pyrazole-3'-carboxylate
;
_journal_coeditor_code           BT4095
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x200945
_journal_paper_doi               10.1107/S2414314620009451
_journal_volume                  5
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C25 H29 Cl N2 O7'
_chemical_formula_moiety         'C25 H29 Cl N2 O7'
_chemical_formula_sum            'C25 H29 Cl N2 O7'
_chemical_formula_weight         504.95
_chemical_name_systematic
'Ethyl 10\a-hydroxy-4,9-dimethyl-14-oxo-3,8,15-trioxatetracyclo[10.3.0.0^2,4^.0^7,9^]pentadecane-13-spiro-5'-pyrazole-3'-carboxylate'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                   9.2324(3)
_cell_length_b                   11.1656(4)
_cell_length_c                   23.3497(8)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.723
_cell_measurement_theta_min      2.524
_cell_volume                     2407.01(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>, 2020) and PublCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'APEX II CCD area-detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 APEX3'
_diffrn_measurement_method       '\f and \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  0.0410
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            72348
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.723
_diffrn_reflns_theta_min         2.524
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6798
_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    1.393
_exptl_crystal_description       Block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.200
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3371 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.009(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         9629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0657P)^2^+0.1273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                8323
_reflns_number_total             9629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4095sup1.cif
_cod_data_source_block           I
_cod_database_code               1558658
_cod_database_fobs_code          1558658
_shelx_hkl_checksum              18278
_shelx_res_checksum              76075