#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:00:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179772 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/68/7006810.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7006810
loop_
_publ_author_name
'Ren, X. M.'
'Nishihara, S.'
'Akutagawa, T.'
'Noro, S.'
'Nakamura, T.'
'Fujita, W.'
'Awaga, K.'
'Ni, Z. P.'
'Xie, J. L.'
'Meng, Q. J.'
'Kremer, R. K.'
_publ_section_title
;
 Quasi-one-dimensional molecular magnets based on derivatives of
 (fluorobenzyl)pyridinium with the [M(mnt)2] monoanion (M = Ni, Pd or
 Pt; mnt2- = maleonitriledithiolate): syntheses, crystal structures and
 magnetic properties.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1988
_journal_page_last               1994
_journal_paper_doi               10.1039/b514278d
_journal_year                    2006
_chemical_formula_sum            'C20 H9 F3 N5 Ni S4'
_chemical_formula_weight         563.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.445(2)
_cell_length_b                   22.234(6)
_cell_length_c                   13.400(5)
_cell_measurement_reflns_used    31525
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2194.3(12)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31084
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0150P)²+1.9719P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                4059
_reflns_number_total             4562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b514278d.txt
_cod_data_source_block           CCDC285872
_cod_database_code               7006810
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.71022(3) 0.971702(10) 0.489994(17) 0.01324(6) Uani 1 1 d . . .
S1 S 0.70683(6) 1.01288(2) 0.34513(3) 0.01657(10) Uani 1 1 d . . .
S2 S 0.83014(6) 1.04951(2) 0.56859(3) 0.01530(10) Uani 1 1 d . . .
S3 S 0.58827(6) 0.894539(19) 0.40963(3) 0.01562(10) Uani 1 1 d . . .
S4 S 0.71820(6) 0.92932(2) 0.63492(3) 0.01545(10) Uani 1 1 d . . .
F1 F 0.33401(14) 0.52635(5) 0.39282(8) 0.0227(2) Uani 1 1 d . . .
F2 F 0.55016(15) 0.43322(5) 0.35685(9) 0.0254(3) Uani 1 1 d . . .
F3 F 0.91017(15) 0.45084(5) 0.35997(9) 0.0258(3) Uani 1 1 d . . .
N1 N 0.8395(2) 1.15237(8) 0.22448(13) 0.0257(4) Uani 1 1 d . . .
N2 N 1.0109(2) 1.19988(7) 0.52188(13) 0.0239(4) Uani 1 1 d . . .
N3 N 0.4487(2) 0.73724(7) 0.46486(13) 0.0223(4) Uani 1 1 d . . .
N4 N 0.6126(2) 0.77951(7) 0.74215(13) 0.0238(4) Uani 1 1 d . . .
N5 N 0.9448(2) 0.66923(6) 0.54504(12) 0.0153(3) Uani 1 1 d . . .
C1 C 0.8235(2) 1.12151(8) 0.29125(15) 0.0179(4) Uani 1 1 d . . .
C2 C 0.8015(2) 1.08200(8) 0.37359(14) 0.0159(4) Uani 1 1 d . . .
C3 C 0.8563(2) 1.09808(8) 0.47207(14) 0.0159(4) Uani 1 1 d . . .
C4 C 0.9415(2) 1.15493(8) 0.49854(14) 0.0171(4) Uani 1 1 d . . .
C5 C 0.5034(2) 0.78515(8) 0.48087(14) 0.0162(4) Uani 1 1 d . . .
C6 C 0.5739(2) 0.84417(8) 0.50502(14) 0.0149(4) Uani 1 1 d . . .
C7 C 0.6312(2) 0.85934(8) 0.60387(14) 0.0150(4) Uani 1 1 d . . .
C8 C 0.6214(2) 0.81592(8) 0.68228(14) 0.0173(4) Uani 1 1 d . . .
C9 C 0.8468(2) 0.66620(9) 0.62229(15) 0.0205(4) Uani 1 1 d . . .
H9A H 0.7235 0.6575 0.6092 0.025 Uiso 1 1 calc R . .
C10 C 0.9271(3) 0.67583(9) 0.71938(16) 0.0259(4) Uani 1 1 d . . .
H10A H 0.8591 0.6735 0.7722 0.031 Uiso 1 1 calc R . .
C11 C 1.1110(3) 0.68921(9) 0.73831(16) 0.0264(4) Uani 1 1 d . . .
H11A H 1.1673 0.6966 0.8038 0.032 Uiso 1 1 calc R . .
C12 C 1.2093(3) 0.69136(9) 0.65851(16) 0.0250(4) Uani 1 1 d . . .
H12A H 1.3330 0.6996 0.6700 0.030 Uiso 1 1 calc R . .
C13 C 1.1234(2) 0.68121(8) 0.56232(15) 0.0197(4) Uani 1 1 d . . .
H13A H 1.1894 0.6826 0.5086 0.024 Uiso 1 1 calc R . .
C14 C 0.8511(2) 0.66330(8) 0.43892(14) 0.0174(4) Uani 1 1 d . . .
H14A H 0.9374 0.6713 0.3929 0.021 Uiso 1 1 calc R . .
H14B H 0.7553 0.6931 0.4268 0.021 Uiso 1 1 calc R . .
C15 C 0.7707(2) 0.60149(8) 0.41780(13) 0.0156(4) Uani 1 1 d . . .
C16 C 0.5843(2) 0.59285(8) 0.41372(14) 0.0169(4) Uani 1 1 d . . .
H16A H 0.5091 0.6249 0.4242 0.020 Uiso 1 1 calc R . .
C17 C 0.5132(2) 0.53625(9) 0.39396(14) 0.0176(4) Uani 1 1 d . . .
C18 C 0.6213(3) 0.48833(8) 0.37588(14) 0.0179(4) Uani 1 1 d . . .
C19 C 0.8057(2) 0.49791(8) 0.37893(14) 0.0180(4) Uani 1 1 d . . .
C20 C 0.8817(2) 0.55352(8) 0.40001(14) 0.0163(4) Uani 1 1 d . . .
H20A H 1.0061 0.5591 0.4024 0.020 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 S2 92.81(3) . . ?
S1 Ni1 S4 178.87(2) . . ?
S2 Ni1 S4 87.45(3) . . ?
S1 Ni1 S3 86.51(3) . . ?
S2 Ni1 S3 179.21(2) . . ?
S4 Ni1 S3 93.24(3) . . ?
C2 S1 Ni1 103.41(7) . . ?
C3 S2 Ni1 102.81(7) . . ?
C6 S3 Ni1 102.43(7) . . ?
C7 S4 Ni1 102.65(7) . . ?
C13 N5 C9 120.61(17) . . ?
C13 N5 C14 119.60(15) . . ?
C9 N5 C14 119.66(15) . . ?
N1 C1 C2 178.9(2) . . ?
C3 C2 C1 121.88(17) . . ?
C3 C2 S1 120.26(14) . . ?
C1 C2 S1 117.85(14) . . ?
C2 C3 C4 121.75(17) . . ?
C2 C3 S2 120.70(14) . . ?
C4 C3 S2 117.53(15) . . ?
N2 C4 C3 178.4(2) . . ?
N3 C5 C6 177.7(2) . . ?
C7 C6 C5 119.66(16) . . ?
C7 C6 S3 120.95(14) . . ?
C5 C6 S3 119.38(14) . . ?
C6 C7 C8 119.92(16) . . ?
C6 C7 S4 120.70(14) . . ?
C8 C7 S4 119.37(14) . . ?
N4 C8 C7 177.3(2) . . ?
N5 C9 C10 120.75(18) . . ?
N5 C9 H9A 119.6 . . ?
C10 C9 H9A 119.6 . . ?
C9 C10 C11 119.33(19) . . ?
C9 C10 H10A 120.3 . . ?
C11 C10 H10A 120.3 . . ?
C12 C11 C10 119.1(2) . . ?
C12 C11 H11A 120.5 . . ?
C10 C11 H11A 120.5 . . ?
C13 C12 C11 119.64(19) . . ?
C13 C12 H12A 120.2 . . ?
C11 C12 H12A 120.2 . . ?
N5 C13 C12 120.60(18) . . ?
N5 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
N5 C14 C15 112.07(14) . . ?
N5 C14 H14A 109.2 . . ?
C15 C14 H14A 109.2 . . ?
N5 C14 H14B 109.2 . . ?
C15 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C20 C15 C16 120.05(17) . . ?
C20 C15 C14 120.03(16) . . ?
C16 C15 C14 119.90(16) . . ?
C17 C16 C15 119.11(17) . . ?
C17 C16 H16A 120.4 . . ?
C15 C16 H16A 120.4 . . ?
F1 C17 C16 120.21(16) . . ?
F1 C17 C18 118.26(17) . . ?
C16 C17 C18 121.53(17) . . ?
F2 C18 C17 120.93(17) . . ?
F2 C18 C19 120.51(16) . . ?
C17 C18 C19 118.56(17) . . ?
F3 C19 C20 120.39(16) . . ?
F3 C19 C18 118.13(16) . . ?
C20 C19 C18 121.49(17) . . ?
C19 C20 C15 119.24(17) . . ?
C19 C20 H20A 120.4 . . ?
C15 C20 H20A 120.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1430(8) . ?
Ni1 S2 2.1505(7) . ?
Ni1 S4 2.1515(8) . ?
Ni1 S3 2.1545(7) . ?
S1 C2 1.7106(19) . ?
S2 C3 1.7176(19) . ?
S3 C6 1.7144(19) . ?
S4 C7 1.7132(19) . ?
F1 C17 1.350(2) . ?
F2 C18 1.344(2) . ?
F3 C19 1.350(2) . ?
N1 C1 1.148(3) . ?
N2 C4 1.147(2) . ?
N3 C5 1.149(2) . ?
N4 C8 1.148(2) . ?
N5 C13 1.343(2) . ?
N5 C9 1.352(2) . ?
N5 C14 1.495(2) . ?
C1 C2 1.438(3) . ?
C2 C3 1.371(3) . ?
C3 C4 1.435(3) . ?
C5 C6 1.433(3) . ?
C6 C7 1.373(3) . ?
C7 C8 1.437(3) . ?
C9 C10 1.367(3) . ?
C9 H9A 0.9300 . ?
C10 C11 1.388(3) . ?
C10 H10A 0.9300 . ?
C11 C12 1.382(3) . ?
C11 H11A 0.9300 . ?
C12 C13 1.371(3) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.509(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C20 1.391(3) . ?
C15 C16 1.394(3) . ?
C16 C17 1.376(3) . ?
C16 H16A 0.9300 . ?
C17 C18 1.378(3) . ?
C18 C19 1.384(3) . ?
C19 C20 1.372(3) . ?
C20 H20A 0.9300 . ?
