Six tris(bipyridyl)iron(II) complexes with 2-substituted 1,1,3,3-tetracyanopropenide, perchlorate and tetrafluoridoborate anions; order <i>versus</i> disorder, hydrogen bonding and C—N···π interactions
Addala, Abderezak; Setifi, Zouaoui; Morimoto, Yukio; Artetxe, Beñat; Matsumoto, Takashi; Gutiérrez-Zorrilla, Juan M.; Glidewell, Christopher; Acta Crystallographica Section E 74 (2018) 1717–1726; doi:10.1107/S2056989018015426

data_2242712
_publ_section_title
;
 Six tris(bipyridyl)iron(II) complexes with 2-substituted
 1,1,3,3-tetracyanopropenide, perchlorate and tetrafluoridoborate anions;
 order <i>versus</i> disorder, hydrogen bonding and
 C---N&#x00B7;&#x00B7;&#x00B7;\p interactions
;
_journal_coeditor_code           SJ5565
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1717
_journal_page_last               1726
_journal_paper_doi               10.1107/S2056989018015426
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Fe (C10 H8 N2)3] (C8 H3 N4 O)2, 0.776H2 O'
_chemical_formula_moiety
'C30 H24 Fe N6 2+, 2(C8 H3 N4 O -), 0.776(H2 O)'
_chemical_formula_sum            'C46 H31.55 Fe N14 O2.78'
_chemical_formula_weight         880.65
_chemical_name_systematic
;
Tris(2,2'-bipyridine)iron(II)
bis(1,1,3,3-tetracyano-2-methoxypropenide) 0.776-hydrate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 97.5030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.3410(3)
_cell_length_b                   11.27560(10)
_cell_length_c                   19.33740(16)
_cell_measurement_reflns_used    7579
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.241
_cell_measurement_theta_min      4.090
_cell_volume                     8288.32(12)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material  'SHELXL2014 and PLATON'
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26027
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         4.090
_diffrn_source                   'sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.419
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       needle
_exptl_crystal_F_000             3630
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         7579
_refine_ls_number_restraints     560
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+3.4626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                6565
_reflns_number_total             7579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5565sup1.cif
_cod_data_source_block           I
_cod_database_code               2242712
_shelx_estimated_absorpt_t_min   0.635
_shelx_estimated_absorpt_t_max   0.935
_shelx_hkl_checksum              97658
_shelx_res_checksum              28289
_shelxl_version_number           2.014
_cod_database_fobs_code 2242712