Crystal structure of 1,4-bis(benzo[d][1,3]dioxol-5-ylmethyl)dihydro-1H,3H-furo[3,4-c]furan-3a(4H)-yl acetate, C22H20O8
Deng, Rui; Zhao, Chen-Liang; Ye, Jiang-Hai; Liu, Ya-Hua; Zou, Juan; Pan, Lu-Tai; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 829–830; doi:10.1515/ncrs-2018-0039

data_8106313
_publ_section_title
;
 Crystal structure of
 1,4-bis(benzo[d][1,3]dioxol-5-ylmethyl)dihydro-1H,3H-furo[3,4-c]furan-3a(4H)-yl
 acetate, C22H20O8
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              829
_journal_page_last               830
_journal_paper_doi               10.1515/ncrs-2018-0039
_journal_volume                  233
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C22 H20 O8'
_chemical_formula_sum            'C22 H20 O8'
_chemical_formula_weight         412.40
_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_Int_Tables_number      4
_cell_angle_alpha                90
_cell_angle_beta                 101.709(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5482(10)
_cell_length_b                   7.0055(9)
_cell_length_c                   18.245(3)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.15
_cell_volume                     944.7(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9693
_diffrn_measured_fraction_theta_max 0.9693
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6183
_diffrn_reflns_theta_full        24.9980
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.9770
_exptl_absorpt_correction_T_min  0.9749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.4497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432.2912
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.1889
_refine_diff_density_min         -0.1620
_refine_diff_density_rms         0.0471
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   9.64(7)
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             17.8654
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0631
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3218
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0631
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.0018
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.933
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              8
_reflns_limit_k_min              -8
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                2704
_reflns_number_total             3218
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2018-0039_suppl.cif
_cod_data_source_block           a
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               8106313
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6), C5(H5), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C4(H4a,H4b), C7''(H7'a,H7'b), C7'(H7'c,H7'd)
2.c Me refined with riding coordinates:
 C10(H10a,H10b,H10c)
2.d Aromatic/amide H refined with riding coordinates:
 C6''(H6''), C6'(H6'), C5'(H5'), C5''(H5''), C2''(H2''), C2'(H2')
;
_olex2_submission_special_instructions 'No special instructions were received'