Crystal structure and Hirshfeld surface analysis of tris(2,2'-bipyridine)nickel(II) bis(1,1,3,3-tetracyano-2-ethoxypropenide) dihydrate
Chi-Duran, Ignacio; Setifi, Zouaoui; Setifi, Fatima; Jelsch, Christian; Morgenstern, Bernd; Vega, Andres; Herrera, Felipe; Pratap Singh, Dinesh; Hegetschweiler, Kaspar; Boyaala, Rabab; Acta Crystallographica Section E 75 (2019) 867–871; doi:10.1107/S2056989019006959

data_2243001
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of
 tris(2,2'-bipyridine)nickel(II) bis(1,1,3,3-tetracyano-2-ethoxypropenide)
 dihydrate
;
_journal_coeditor_code           MW2141
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              867
_journal_page_last               871
_journal_paper_doi               10.1107/S2056989019006959
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ni (C10 H8 N2)3] (C9 H5 N4 O)2, 2H2 O'
_chemical_formula_moiety         'C30 H24 N6 Ni 2+, 2(C9 H5 N4 O -), 2(H2 O)'
_chemical_formula_sum            'C48 H38 N14 Ni O4'
_chemical_formula_weight         933.63
_chemical_name_systematic
;
Tris(2,2'-bipyridine)nickel(II)
bis(1,1,3,3-tetracyano-2-ethoxypropenide)
dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 112.800(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.345(3)
_cell_length_b                   12.439(3)
_cell_length_c                   19.575(4)
_cell_measurement_reflns_used    1400
_cell_measurement_temperature    162(2)
_cell_measurement_theta_max      19.05
_cell_measurement_theta_min      2.45
_cell_volume                     4566.8(16)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      162(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.1339
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22477
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.451
_diffrn_reflns_theta_min         1.965
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.395
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4670
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+4.4221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                2483
_reflns_number_total             4670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2141sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4566.8(17)
_cod_database_code               2243001
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.966
_shelx_hkl_checksum              44393
_shelx_res_checksum              11030
_shelxl_version_number           2014/6
_cod_database_fobs_code 2243001