Crystal structure of (9<i>S</i>,10<i>S</i>)-10-ethoxy-9-hydroxy-6,6,9-trimethyl-3-pentyl-7,8,9,10-tetrahydro-6<i>H</i>-benzo[<i>c</i>]chromen-1-yl 4-methylbenzenesulfonate
Gul, Waseem; Galal, Ahmed; ElSohly, Mahmoud A.; Carvalho, Paulo; Acta Crystallographica Section E 71 (2015) o1082–o1083; doi:10.1107/S2056989015024044

data_2241494
_publ_section_title
;
 Crystal structure of
 (9<i>S</i>,10<i>S</i>)-10-ethoxy-9-hydroxy-6,6,9-trimethyl-3-pentyl-7,8,9,10-tetrahydro-6<i>H</i>-benzo[<i>c</i>]chromen-1-yl
 4-methylbenzenesulfonate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1082
_journal_page_last               o1083
_journal_paper_doi               10.1107/S2056989015024044
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C30 H40 O6 S'
_chemical_formula_moiety         'C30 H40 O6 S'
_chemical_formula_sum            'C30 H40 O6 S'
_chemical_formula_weight         528.68
_chemical_name_systematic
'(9<i>S</i>,10<i>S</i>)-10-Ethoxy-9-hydroxy-6,6,9-trimethyl-3-pentyl-7,8,9,10-tetrahydro-6<i>H</i>-benzo[<i>c</i>]chromen-1-yl 4-methylbenzenesulfonate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9090(10)
_cell_length_b                   10.2373(10)
_cell_length_c                   13.8402(10)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.05
_cell_measurement_theta_min      4.546
_cell_volume                     1378.2(2)
_computing_cell_refinement
;
SAINT (Bruker, 2000)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008), ORTEP3 for Windows (Farrugia,
2012), POV-RAY
(Cason, 2003)
;
_computing_publication_material
;
ENCIFER (Allen <i>et al.</i>,  2004), publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21062
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.146
_diffrn_reflns_theta_min         3.253
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.275
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4984
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0429P)^2^+0.1558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                4834
_reflns_number_total             4984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tk5416sup1.cif
_cod_data_source_block           I
_cod_database_code               2241494
_cod_database_fobs_code          2241494
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.779
_shelx_hkl_checksum              31684
_shelx_res_checksum              97975