(4<i>R</i>,4a<i>R</i>,6<i>S</i>,7<i>S</i>,7a<i>S</i>)-6-Hydroxy-7-hydroxymethyl-4-methylperhydrocyclopenta[<i>c</i>]pyran-1-one chloroform solvate from <i>Valeriana laxiflora</i>
Khera, Smriti; Carducci, Michael D.; Gu, Jian-Qiao; Timmermann, Barbara N.; Acta Crystallographica Section C 60 (2004) o773–o775; doi:10.1107/S0108270104021511

data_2014572
_publ_section_title
;(4<i>R</i>,4a<i>R</i>,6<i>S</i>,7<i>S</i>,7a<i>S</i>)-6-Hydroxy-7-hydroxymethyl-4-methylperhydrocyclopenta[<i>c</i>]pyran-1-one
 chloroform solvate from <i>Valeriana laxiflora</i>
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o773
_journal_page_last               o775
_journal_paper_doi               10.1107/S0108270104021511
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C10 H16 O4, C H Cl3'
_chemical_formula_moiety         'C10 H16 O4, C H Cl3'
_chemical_formula_sum            'C11 H17 Cl3 O4'
_chemical_formula_weight         319.60
_chemical_melting_point          .91E-91
_chemical_name_systematic
;(4R,5R,7S,8S,9S)-7-hydroxy-8-hydroxymethyl-4-methyl-perhydrocyclopenta[c]pyran-
1-one
 chloroform solvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 94.478(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.523(3)
_cell_length_b                   6.0404(15)
_cell_length_c                   11.231(3)
_cell_measurement_reflns_used    794
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.76
_cell_measurement_theta_min      2.55
_cell_volume                     711.7(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0883
_diffrn_reflns_av_sigmaI/netI    0.1261
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6446
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_time  1200
_diffrn_standards_number         58
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_correction_T_min  0.2677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.264
_refine_ls_abs_structure_details 'Flack (1983), 1032 Friedel pairs'
_refine_ls_abs_structure_Flack   0.11(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2420
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                1504
_reflns_number_total             2420
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sx1145.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2014572
_cod_database_fobs_code          2014572