Crystal structure of dimethyl (3aS,6R,6aS,7S)-2-pivaloyl-2,3-dihydro-1H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isoquinoline-3a1,6a-dicarboxylate, C21H25NO8
Dorovatovskii, Pavel V.; Sadigova, Nurlana D.; Huseynzada, Alakbar E.; Hajiyeva, Sarvinaz F.; Cárdenas, Alejandro; Cisterna, Jonathan; Brito, Iván; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 205–207; doi:10.1515/ncrs-2018-0192

data_8105591
_publ_section_title
;
 Crystal structure of dimethyl
 (3aS,6R,6aS,7S)-2-pivaloyl-2,3-dihydro-1H,6H,7H-3a,6:7,9a-diepoxybenzo[de]isoquinoline-3a1,6a-dicarboxylate,
 C21H25NO8
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              205
_journal_page_last               207
_journal_paper_doi               10.1515/ncrs-2018-0192
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C21 H25 N O8'
_chemical_formula_sum            'C21 H25 N O8'
_chemical_formula_weight         419.42
_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                 118.19(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.905(3)
_cell_length_b                   13.370(3)
_cell_length_c                   13.090(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1990.7(10)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Synchrotron Radiation '
_diffrn_radiation_type           'Synchrotron Radiation'
_diffrn_radiation_wavelength     0.9699
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.912
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21424
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.508
_diffrn_reflns_theta_min         4.160
_exptl_absorpt_coefficient_mu    0.252
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.018(2)
_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   1.362
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.362
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0690P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1966
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2857
_reflns_number_total             4031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0192_suppl.cif
_cod_data_source_block           ek13
_cod_original_cell_volume        1990.5(8)
_cod_database_code               8105591
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.951
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.032) H1B(0.032) H3A(0.033) H3B(0.033) H4(0.035) H5(0.037)
 H6(0.034) H7(0.033) H8(0.031) H9(0.03) H12A(0.063) H12B(0.063) H12C(0.063)
 H13A(0.056) H13B(0.056) H13C(0.056) H14A(0.069) H14B(0.069) H14C(0.069)
 H16A(0.058) H16B(0.058) H16C(0.058) H18A(0.051) H18B(0.051) H18C(0.051)
 Fixed X: H1A(0.59513) H1B(0.607045) H3A(0.463968) H3B(0.381142) H4(0.526204)
 H5(0.627273) H6(0.645004) H7(0.78047) H8(0.947277) H9(0.85488) H12A(0.272911)
 H12B(0.158281) H12C(0.281257) H13A(0.199281) H13B(0.07215) H13C(0.128905)
 H14A(0.108058) H14B(0.05133) H14C(0.166119) H16A(0.969886) H16B(1.036385)
 H16C(0.973921) H18A(0.654694) H18B(0.784086) H18C(0.692729)
 Fixed Y: H1A(0.420758) H1B(0.54019) H3A(0.64092) H3B(0.576736) H4(0.739848)
 H5(0.676562) H6(0.487444) H7(0.361709) H8(0.401213) H9(0.476216)
 H12A(0.248818) H12B(0.214061) H12C(0.22531) H13A(0.349841) H13B(0.336168)
 H13C(0.445317) H14A(0.475482) H14B(0.367574) H14C(0.400875) H16A(0.705079)
 H16B(0.672011) H16C(0.779088) H18A(0.876343) H18B(0.829329) H18C(0.801415)
 Fixed Z: H1A(0.4829) H1B(0.491118) H3A(0.308017) H3B(0.195366) H4(0.148393)
 H5(0.041309) H6(0.068482) H7(0.257709) H8(0.460299) H9(0.571544)
 H12A(0.099988) H12B(0.107969) H12C(0.223532) H13A(0.312616) H13B(0.20291)
 H13C(0.238635) H14A(0.044112) H14B(-0.001534) H14C(-0.010054) H16A(0.205033)
 H16B(0.338315) H16C(0.302933) H18A(0.425467) H18B(0.486658) H18C(0.53261)
;