Crystal structure of [tris(4,4'-bipyridine)]diium bis(1,1,3,3-tetracyano-2-ethoxypropenide) trihydrate
Setifi, Fatima; Valkonen, Arto; Setifi, Zouaoui; Nummelin, Sami; Touzani, Rachid; Glidewell, Christopher; Acta Crystallographica Section E 72 (2016) 1246–1250; doi:10.1107/S2056989016012160

data_2241803
_publ_section_title
;
 Crystal structure of [tris(4,4'-bipyridine)]diium
 bis(1,1,3,3-tetracyano-2-ethoxypropenide) trihydrate
;
_journal_coeditor_code           HB7603
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1246
_journal_page_last               1250
_journal_paper_doi               10.1107/S2056989016012160
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C30 H26 N6 2+, 2C9 H5 N4 O -, 3H2 O'
_chemical_formula_moiety         'C30 H26 N6 2+, 2(C9 H5 N4 O -), 3(H2 O)'
_chemical_formula_sum            'C48 H42 N14 O5'
_chemical_formula_weight         894.95
_chemical_name_systematic
;
[Tris(4,4-bipyridine)]diium
bis(1,1,3,3-tetracyano-2-ethoxypropenide) trihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 100.4480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1861(2)
_cell_length_b                   7.11870(10)
_cell_length_c                   35.7070(4)
_cell_measurement_reflns_used    5197
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.32
_cell_volume                     4546.03(10)
_computing_cell_refinement
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Bruker, 2008)
;
_computing_data_reduction
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker--Nonius Kappa CCD with APEXII detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            35680
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         2.320
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.310
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5197
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0362P)^2^+5.2868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                4559
_reflns_number_total             5197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7603sup1.cif
_cod_data_source_block           I
_cod_database_code               2241803
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.973
_shelx_hkl_checksum              28612
_shelx_res_checksum              14478
_shelxl_version_number           2.014
_cod_database_fobs_code 2241803