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_2242715
_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 (C12 H12 N2)3] (C9 H5 N4 O) (B F4)'
_chemical_formula_moiety         'C36 H36 Fe N6 2+, C9 H5 N4 O -, B F4 -'
_chemical_formula_sum            'C45 H41 B F4 Fe N10 O'
_chemical_formula_weight         880.54
_chemical_name_systematic
;
Tris(5,5'-dimethyl-2,2'-bipyridine)iron(II)
1,1,3,3-tetracyano-2-ethoxypropenide tetrafluoridoborate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 104.641(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5865(3)
_cell_length_b                   25.5914(5)
_cell_length_c                   14.4997(3)
_cell_measurement_reflns_used    7609
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.251
_cell_measurement_theta_min      4.306
_cell_volume                     4159.77(17)
_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  0.0786
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30853
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         4.306
_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    3.475
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       needle
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.706
_refine_diff_density_min         -0.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         7607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0959P)^2^+0.2678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1620
_reflns_number_gt                5392
_reflns_number_total             7607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5565sup1.cif
_cod_data_source_block           IV
_cod_database_code               2242715
_cod_database_fobs_code          2242715
_shelx_estimated_absorpt_t_min   0.649
_shelx_estimated_absorpt_t_max   0.921
_shelx_hkl_checksum              39059
_shelx_res_checksum              51239
_shelxl_version_number           2.014