Potassium (1-methoxycarbonyl-2-methylprop-2-en-2-ylidene)azinate
Reuter, Cédric; Neudörfl, Jörg M.; Schmalz, Hans-Günther; Acta Crystallographica Section E 66 (2010) m461–; doi:10.1107/S1600536810010159

data_2225619
_publ_section_title
;
 Potassium (1-methoxycarbonyl-2-methylprop-2-en-2-ylidene)azinate
;
_journal_coeditor_code           JJ2024
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m461
_journal_paper_doi               10.1107/S1600536810010159
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'K +, C6 H8 N O4 -'
_chemical_formula_moiety         'K +, C6 H8 N O4 -'
_chemical_formula_sum            'C6 H8 K N O4'
_chemical_formula_weight         197.23
_chemical_melting_point          180.7(10)
_chemical_name_systematic
;
Potassium (1-methoxycarbonyl-2-methylprop-2-en-2-ylidene)azinate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.361(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.9269(13)
_cell_length_b                   5.2909(2)
_cell_length_c                   14.2510(7)
_cell_measurement_reflns_used    6264
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      1.85
_cell_volume                     1656.21(14)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SCHAKAL99 (Keller, 1999)'
_computing_publication_material
;
PLATON (Spek, 2009), publCIF (Westrip, 2010) and ORTEP
(Davenport <i>et al.</i>,  1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       Phi/Omega-Scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6264
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platlet
_exptl_crystal_F_000             816
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .03
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                1416
_reflns_number_total             1810
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jj2024.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C m 2/c'
_cod_database_code               2225619
_cod_database_fobs_code          2225619