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_7155022
_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         'C36 H22 N8 O6 Rb2'
_chemical_formula_sum            'C36 H22 N8 O6 Rb2'
_chemical_formula_weight         833.55
_chemical_name_systematic
;
 rubidium 1,1,3,3-tetracyano-2-(2-(isopropoxycarbonyl)benzoyl)prop-2-en-1-ide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_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                 108.37(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.935(4)
_cell_length_b                   7.888(2)
_cell_length_c                   18.793(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      14
_cell_volume                     3648.7(15)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      298(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     0.1231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.518
_diffrn_reflns_point_group_measured_fraction_max 0.517
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.967
_diffrn_reflns_theta_min         1.655
_exptl_absorpt_coefficient_mu    2.739
_exptl_absorpt_correction_T_max  0.7604
_exptl_absorpt_correction_T_min  0.4852
_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    1.518
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1664
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: propanol-2'
_exptl_crystal_size_max          .23
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .11
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.011(14)
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         3695
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.034
_reflns_Friedel_fraction_full    0.035
_reflns_Friedel_fraction_max     0.034
_reflns_number_gt                1959
_reflns_number_total             3695
_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        3648.4(15)
_cod_database_code               7155022
_exptl_absorpt_factor_mur        0.274
_shelxl_version_number           2013-4
_shelx_res_checksum              75932