Supramolecular complexes involving non-symmetric viologen cations and hexacyanoferrate(II) anions. A spectroscopic, crystallographic and computational study.
Papadakis, Raffaello; Deligkiozi, Ioanna; Giorgi, Michel; Faure, Bruno; Tsolomitis, Athanase; RSC Advances 6 (2015) 575–585; doi:10.1039/C5RA16732A

data_7223536
_publ_section_title
;
 Supramolecular complexes involving non-symmetric viologen cations and
 hexacyanoferrate(II) anions. A spectroscopic, crystallographic and
 computational study.
;
_journal_coden_ASTM              RSCACL
_journal_issue                   1
_journal_name_full               'RSC Advances'
_journal_page_first              575
_journal_page_last               585
_journal_paper_doi               10.1039/C5RA16732A
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         '4(C18 H18 N2), 2(C6 Fe N6), 8.75(H2 O)'
_chemical_formula_sum            'C84 H89.5 Fe2 N20 O8.75'
_chemical_formula_weight         1630.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-29 deposited with the CCDC.
2015-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6547(5)
_cell_length_b                   34.5808(13)
_cell_length_c                   35.0669(11)
_cell_measurement_reflns_used    13998
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2690
_cell_measurement_theta_min      3.6090
_cell_volume                     17770.9(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -72.00   48.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0728  -77.0000 -120.0000 120

  2 omega  -24.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0728   77.0000 -180.0000 120

  3 omega  -20.00   21.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.9791  -99.0000   30.0000 41

  4 omega -104.00  -57.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.9791 -178.0000   60.0000 47

  5 omega  -19.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0728   38.0000    0.0000 110

  6 omega  -20.00   56.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0728  -99.0000   60.0000 76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0085773000
_diffrn_orient_matrix_UB_12      0.0177367000
_diffrn_orient_matrix_UB_13      0.0095105000
_diffrn_orient_matrix_UB_21      0.0080087000
_diffrn_orient_matrix_UB_22      0.0091278000
_diffrn_orient_matrix_UB_23      -0.0178010000
_diffrn_orient_matrix_UB_31      -0.0469630000
_diffrn_orient_matrix_UB_32      0.0047842500
_diffrn_orient_matrix_UB_33      -0.0013008500
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            87803
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_F_000             6844
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 4498 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1107
_refine_ls_number_reflns         15088
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0875
_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^)+(0.1892P)^2^+10.2930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2420
_refine_ls_wR_factor_ref         0.2694
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                11405
_reflns_number_total             15088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra16732a2.cif
_cod_data_source_block           viologenmo
_cod_original_formula_sum        'C84 H89.50 Fe2 N20 O8.75'
_cod_database_code               7223536
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C77-C78
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C74 \\sim C75 \\sim C76 \\sim C77: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O5) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O10)
\\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
4. Others
 Fixed Sof: H85A(0.5) H85B(0.5) H85C(0.5) H90A(0.5) H90B(0.5) H90C(0.5)
 H73A(0.5) H73B(0.5) H73C(0.5) H78A(0.5) H78B(0.5) H78C(0.5) O8(0.5) H8A(0.5)
 H8B(0.5) O9(0.25) H9A(0.25) H9B(0.25) O7(0.25) H7A(0.25) H7B(0.25) O5(0.5)
 H5A(0.5) H5B(0.5) O3(0.25) H3A(0.25) H3B(0.25) O6(0.25) H6A(0.25) H6B(0.25)
 O4(0.25) H4A(0.25) H4B(0.25) O12(0.5) H12A(0.5) H12B(0.5) O13(0.5) H13A(0.5)
 H13B(0.5) O14(0.5) H14A(0.5) H14B(0.5) O15(0.5) H15A(0.5) H15B(0.5) O16(0.5)
 H16A(0.5) H16B(0.5)
5.a Riding coordinates:
 O8(H8A,H8B), O9(H9A,H9B), O7(H7A,H7B), O5(H5A,H5B), O3(H3A,H3B), O1(H1A,H1B),
 O6(H6A,H6B), O4(H4A,H4B), O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B),
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O10(H10A,H10B), O11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C50(H50), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57),
 C58(H58), C61(H61), C62(H62), C64(H64), C65(H65), C13(H13), C14(H14), C16(H16),
  C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26),
 C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38),
  C39(H39), C40(H40), C43(H43), C44(H44), C46(H46), C47(H47), C79(H79),
 C80(H80), C83(H83), C84(H84), C87(H87), C88(H88), C67(H67), C68(H68), C71(H71),
  C72(H72), C75(H75), C76(H76)
5.c Idealised Me refined with riding coordinates:
 C59(H59A,H59B,H59C), C66(H66A,H66B,H66C), C23(H23A,H23B,H23C), C30(H30A,H30B,
 H30C), C41(H41A,H41B,H41C), C48(H48A,H48B,H48C), C85(H85A,H85B,H85C), C90(H90A,
 H90B,H90C), C73(H73A,H73B,H73C), C78(H78A,H78B,H78C)
;
_olex2_submission_special_instructions 'No special instructions were received'