Crystal structure of dimethyl (3aS,6R,6aS,7S)-1H,3H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isochromene-3a 1,6a-dicarboxylate, C16H16O7
Dorovatovskii, Pavel V.; Sadigova, Nurlana D.; Cárdenas, Alejandro; Cisterna, Jonathan; Brito, Iván; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 1075–1077; doi:10.1515/ncrs-2018-0195

data_8106405
_publ_section_title
;
 Crystal structure of dimethyl
 (3aS,6R,6aS,7S)-1H,3H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isochromene-3a
 1,6a-dicarboxylate, C16H16O7
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1075
_journal_page_last               1077
_journal_paper_doi               10.1515/ncrs-2018-0195
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C16 H16 O7'
_chemical_formula_sum            'C16 H16 O7'
_chemical_formula_weight         320.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 114.88(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.830(3)
_cell_length_b                   8.1101(16)
_cell_length_c                   14.900(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1406.5(6)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_radiation_type           'synchroton radiation'
_diffrn_radiation_wavelength     0.9699
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_unetI/netI     0.1010
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13125
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.487
_diffrn_reflns_theta_min         3.751
_exptl_absorpt_coefficient_mu    0.282
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.518
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.518
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0329P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2293
_reflns_number_total             3051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0195_suppl.cif
_cod_data_source_block           xb12
_cod_database_code               8106405
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.933
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.024) H1B(0.024) H3A(0.024) H3B(0.024) H4(0.02) H5(0.021)
 H6(0.02) H7(0.022) H8(0.024) H9(0.024) H11A(0.032) H11B(0.032) H11C(0.032)
 H13A(0.042) H13B(0.042) H13C(0.042)
 Fixed X: H1A(0.557699) H1B(0.532417) H3A(0.361011) H3B(0.283276) H4(0.128009)
 H5(0.001691) H6(0.088478) H7(0.282245) H8(0.432604) H9(0.559281)
 H11A(0.048904) H11B(0.013231) H11C(0.138885) H13A(0.235775) H13B(0.338625)
 H13C(0.35968)
 Fixed Y: H1A(0.735234) H1B(0.853153) H3A(1.033878) H3B(1.02856) H4(0.991704)
 H5(0.745159) H6(0.535838) H7(0.331857) H8(0.286106) H9(0.531507)
 H11A(0.347361) H11B(0.199667) H11C(0.203744) H13A(0.955633) H13B(0.825145)
 H13C(1.001489)
 Fixed Z: H1A(0.800019) H1B(0.70697) H3A(0.6515) H3B(0.711962) H4(0.492368)
 H5(0.444519) H6(0.583817) H7(0.646628) H8(0.578856) H9(0.623734)
 H11A(0.289415) H11B(0.34204) H11C(0.344019) H13A(0.291368) H13B(0.322623)
 H13C(0.375553)
;
_shelx_res_checksum              16678
_shelx_hkl_checksum              83637
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n