Crystal structures of 4-methyl-2-oxo-2<i>H</i>-chromene-7,8-diyl diacetate and 4-methyl-2-oxo-2<i>H</i>-chromene-7,8-diyl bis(pent-4-ynoate)
Akinyemi, Akintunde; Thomas, Courtney; Marsh, Willis; Butcher, Ray J.; Jasinski, Jerry P.; Maynard-Smith, Lystranne A.; Acta Crystallographica Section E 72 (2016) 704–708; doi:10.1107/S2056989016005892

data_2241660
_publ_section_title
;
 Crystal structures of 4-methyl-2-oxo-2<i>H</i>-chromene-7,8-diyl
 diacetate and 4-methyl-2-oxo-2<i>H</i>-chromene-7,8-diyl
 bis(pent-4-ynoate)
;
_journal_coeditor_code           HG5471
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              704
_journal_page_last               708
_journal_paper_doi               10.1107/S2056989016005892
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C14 H12 O6'
_chemical_formula_moiety         'C14 H12 O6'
_chemical_formula_sum            'C14 H12 O6'
_chemical_formula_weight         276.24
_chemical_name_systematic
;
4-Methyl-2-oxo-2<i>H</i>-chromene-7,8-diyl diacetate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                69.263(10)
_cell_angle_beta                 87.519(11)
_cell_angle_gamma                69.113(10)
_cell_formula_units_Z            2
_cell_length_a                   7.3722(10)
_cell_length_b                   8.7235(7)
_cell_length_c                   11.7032(15)
_cell_measurement_reflns_used    1905
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.7690
_cell_measurement_theta_min      4.3510
_cell_volume                     654.66(15)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0416
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Agilent Xcalibur Eos Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7360
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         32.669
_diffrn_reflns_theta_min         3.194
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4296
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0738P)^2^+0.0282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1555
_reflns_number_gt                3087
_reflns_number_total             4296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hg5471sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        654.66(14)
_cod_database_code               2241660
_cod_database_fobs_code          2241660
_shelx_hkl_checksum              99978
_shelx_res_checksum              58599