Acetic anhydride at 100K: the first crystal structure determination
Seidel, Rüdiger W.; Goddard, Richard; Nöthling, Nils; Lehmann, Christian W.; Acta Crystallographica Section C 72 (2016) 753–757; doi:10.1107/S2053229616015047

data_2020594
_publ_section_title
;
 Acetic anhydride at 100K: the first crystal structure determination
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_journal_coeditor_code           YF3110
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              753
_journal_page_last               757
_journal_paper_doi               10.1107/S2053229616015047
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C4 H6 O3'
_chemical_formula_moiety         'C4 H6 O3'
_chemical_formula_sum            'C4 H6 O3'
_chemical_formula_weight         102.09
_chemical_name_common            'Acetic anhydride'
_chemical_name_systematic        'Ethanoic anhydride'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0707(14)
_cell_length_b                   7.8733(13)
_cell_length_c                   7.9305(13)
_cell_measurement_reflns_used    1147
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.0855
_cell_measurement_theta_min      5.4813
_cell_volume                     503.93(15)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2014)
;
_computing_publication_material
;
enCIFer (Allen <i>et al.</i>,  2004)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.67
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker AXS X8 Proteum'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  'MONTEL graded multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            19642
_diffrn_reflns_theta_full        67.371
_diffrn_reflns_theta_max         67.371
_diffrn_reflns_theta_min         7.862
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.66846
_exptl_absorpt_correction_T_min  0.47191
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             216
_exptl_crystal_size_max          1.317
_exptl_crystal_size_mid          0.503
_exptl_crystal_size_min          0.500
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.143
_refine_ls_extinction_coef       0.012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0276P)^2^+0.1605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                445
_reflns_number_total             452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yf3110sup1.cif
_cod_data_source_block           I
_cod_database_code               2020594
_cod_database_fobs_code          2020594
_shelx_estimated_absorpt_t_min   0.349
_shelx_estimated_absorpt_t_max   0.631
_shelx_hkl_checksum              77617
_shelx_res_checksum              56213