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_2241661
_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_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          'C20 H16 O6'
_chemical_formula_moiety         'C20 H16 O6'
_chemical_formula_sum            'C20 H16 O6'
_chemical_formula_weight         352.33
_chemical_name_systematic
;
4-Methyl-2-oxo-2<i>H</i>-chromene-7,8-diyl bis(pent-4-ynoate)
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.992(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.2785(3)
_cell_length_b                   16.3785(8)
_cell_length_c                   20.0502(11)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.361
_cell_measurement_theta_min      2.487
_cell_volume                     1723.95(16)
_computing_cell_refinement
;
APEX2 (Bruker, 2005)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_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      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            24358
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.571
_diffrn_reflns_theta_min         2.487
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       rod
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         5276
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0483P)^2^+1.0298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                3859
_reflns_number_total             5276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hg5471sup1.cif
_cod_data_source_block           2
_cod_database_code               2241661
_cod_database_fobs_code          2241661
_shelx_hkl_checksum              91991
_shelx_res_checksum              44749