Coupling of the lactone-ring conformation with crystal symmetry in 6-hydroxy-4,4,5,7,8-pentamethyl-3,4-dihydrocoumarin
Budzianowski, Armand; Katrusiak, Andrzej; Acta Crystallographica Section B 58 (2002) 125–133; doi:10.1107/S0108768101017955

data_2103159
_publ_section_title
;
 Coupling of the lactone-ring conformation with crystal symmetry in
 6-hydroxy-4,4,5,7,8-pentamethyl-3,4-dihydrocoumarin
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              125
_journal_page_last               133
_journal_paper_doi               10.1107/S0108768101017955
_journal_volume                  58
_journal_year                    2002
_chemical_formula_sum            'C14 H18 O3'
_chemical_formula_weight         234.28
_chemical_name_systematic
;
 6-hydroxy-4,4,5,6,7-pentamethyl-3,4-dihydrocoumarin
;
_space_group_IT_number           14
_symmetry_cell_setting           P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.739(2)
_cell_length_b                   6.895(2)
_cell_length_c                   19.066(5)
_cell_measurement_temperature    277.90(10)
_cell_volume                     1276.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      277.90(10)
_diffrn_measured_fraction_theta_full .910
_diffrn_measured_fraction_theta_max .910
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0546
_diffrn_reflns_av_sigmaI/netI    .1514
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7992
_diffrn_reflns_theta_full        29.41
_diffrn_reflns_theta_max         29.41
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    .085
_exptl_crystal_colour            colourlees
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             504
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .12
_refine_diff_density_max         .148
_refine_diff_density_min         -.124
_refine_ls_extinction_coef       .0055(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   .823
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .823
_refine_ls_R_factor_all          .2414
_refine_ls_R_factor_gt           .0578
_refine_ls_shift/su_max          1.707
_refine_ls_shift/su_mean         .107
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .0957
_refine_ls_wR_factor_ref         .1280
_reflns_number_gt                892
_reflns_number_total             3226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm0046.cif
_cod_data_source_block           cum278
_cod_original_sg_symbol_H-M      monoclinic
_cod_database_code               2103159