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_2242713
_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] (C10 H7 N4 S) (Cl O4)'
_chemical_formula_moiety         'C30 H24 Fe N6 2+, C10 H7 N4 S -, Cl O4 -'
_chemical_formula_sum            'C40 H31 Cl Fe N10 O4 S'
_chemical_formula_weight         839.11
_chemical_name_systematic
;
Tris(2,2'-bipyridine)iron(II) 1,1,3,3-tetracyano-2-(propylsulfanyl)propenide
perchlorate
;
_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                 97.202(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6644(3)
_cell_length_b                   23.1692(4)
_cell_length_c                   13.9599(3)
_cell_measurement_reflns_used    8586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.296
_cell_measurement_theta_min      1.713
_cell_volume                     3742.96(14)
_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
;
<i>Olex2.solve</i> (Dolomanov <i>et al.</i>,  2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.296
_diffrn_reflns_theta_min         1.713
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_refine_diff_density_max         2.234
_refine_diff_density_min         -0.423
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         8586
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0654P)^2^+4.7746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                5903
_reflns_number_total             8586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5565sup1.cif
_cod_data_source_block           II
_cod_database_code               2242713
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.907
_shelx_hkl_checksum              53794
_shelx_res_checksum              93654
_shelxl_version_number           2.014
_cod_database_fobs_code 2242713