Alkali metal complexes of 6-methyl-2-pyridone: simple formulae, but not so simple structures
Clegg, William; Tooke, Duncan M.; Acta Crystallographica Section B 69 (2013) 603–612; doi:10.1107/S2052519213025980

data_2105695
_publ_section_title
;
 Alkali metal complexes of 6-methyl-2-pyridone: simple formulae, but not
 so simple structures
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              603
_journal_page_last               612
_journal_paper_doi               10.1107/S2052519213025980
_journal_volume                  69
_journal_year                    2013
_chemical_formula_moiety         'Cs +,C6 H6 N O -,C2 H6 O'
_chemical_formula_sum            'C8 H12 Cs N O2'
_chemical_formula_weight         287.09
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 100.7564(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.6376(10)
_cell_length_b                   24.980(2)
_cell_length_c                   7.2431(6)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.41
_cell_volume                     2068.6(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  SHELXL-2013
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18269
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         1.781
_exptl_absorpt_coefficient_mu    3.544
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.864
_refine_ls_extinction_coef       0.00039(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+3.5254P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                4243
_reflns_number_total             5014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ps5030.cif
_cod_data_source_block           dmt29_6
_cod_depositor_comments
;

2019-10-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C16 H24 Cs2 N2 O4'
_cod_original_formula_weight         574.19
_cod_original_formula_units_Z            4
_cod_original_cell_volume        2068.7(3)
_cod_database_code               2105695
_shelx_estimated_absorpt_t_min   0.331
_shelx_estimated_absorpt_t_max   0.932
_shelx_hkl_checksum              86958
_shelx_res_checksum              41865
_shelxl_version_number           20.13