Synthesis of novel polycyano-containing organic ligands via double carbanion cleavage of 1',3'-dioxo-1',3'-dihydrospiro[cyclopropane-1,2'-indene] derivatives.
Karpov, S. V.; Kaukov, Ya S.; Grigor'ev, A. A.; Nasakin, O. E.; Kaukova, O. V.; Tafeenko, V. A.; Organic & biomolecular chemistry 14 (2016) 3758–3764; doi:10.1039/c6ob00092d

data_7155023
_publ_section_title
;
 Synthesis of novel polycyano-containing organic ligands via double
 carbanion cleavage of
 1',3'-dioxo-1',3'-dihydrospiro[cyclopropane-1,2'-indene] derivatives.
;
_journal_issue                   15
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3758
_journal_page_last               3764
_journal_paper_doi               10.1039/c6ob00092d
_journal_volume                  14
_journal_year                    2016
_chemical_formula_moiety         'C18 H13 K N2 O7'
_chemical_formula_sum            'C18 H13 K N2 O7'
_chemical_formula_weight         408.40
_chemical_name_systematic
;
 potassium (Z)-2,4-dicyano-1,5-dimethoxy-3-(2-(methoxycarbonyl)benzoyl)-1,5-dioxopent-3-en-2-ide
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-21 deposited with the CCDC.
2016-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.498(5)
_cell_length_b                   13.886(4)
_cell_length_c                   18.696(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      13
_cell_volume                     3763.9(19)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.965
_diffrn_reflns_theta_min         2.179
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.6614
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       prism
_exptl_crystal_F_000             1680
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4085
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0528P)^2^+0.7826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2507
_reflns_number_total             4085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ob00092d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7155021--7155023.cif.'
_cod_original_cell_volume        3764.1(18)
_cod_database_code               7155023
_exptl_absorpt_factor_mur        0.031
_shelxl_version_number           2013-4
_shelx_res_checksum              72551