#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:50:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179734 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/30/7003066.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_7003066
loop_
_publ_author_name
'Ju, Zhan-Feng'
'Yao, Qing-Xia'
'Wu, Wei'
'Zhang, Jie'
_publ_section_title
;
 Strong electron-accepting methylviologen dication confined in magnetic
 hosts: synthesis, structural characterization, charge-transfer and
 magnetic properties of {(MV)2[Ni(SCN)5]·Cl·2H2O}n and
 {(MV)[M(N3)2(SCN)2]}n (M = Mn, Co)
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              355
_journal_paper_doi               10.1039/b710628a
_journal_year                    2008
_chemical_formula_sum            'C29 H32 Cl N9 Ni O2 S5'
_chemical_formula_weight         793.10
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 96.5790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.4118(2)
_cell_length_b                   23.7160(6)
_cell_length_c                   12.1682(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1838.14(9)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10093
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.8737
_exptl_absorpt_correction_T_min  0.7085
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Siemens SMART'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0677P)²+3.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                3206
_reflns_number_total             3573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b710628a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               7003066
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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 0.23627(10) 0.2500 0.95551(5) 0.0387(2) Uani 1 2 d S . .
Cl1 Cl 0.0000 0.0000 0.5000 0.1320(12) Uani 1 2 d S . .
S1 S 0.2627(3) 0.04740(6) 0.94924(13) 0.0948(5) Uani 1 1 d . . .
S2 S -0.1784(2) 0.2500 0.59771(11) 0.0512(4) Uani 1 2 d S . .
S3 S -0.0905(2) 0.2500 1.04969(12) 0.0568(4) Uani 1 2 d S . .
S4 S 0.4852(3) 0.2500 1.34650(12) 0.0620(4) Uani 1 2 d S . .
O1W O -0.2008(7) -0.00916(16) 0.3318(4) 0.0297(9) Uani 0.50 1 d P . .
O1W' O -0.3537(14) 0.0028(3) 0.2964(6) 0.076(2) Uani 0.50 1 d P . .
N1 N -0.0826(7) 0.11456(16) 0.2013(3) 0.0608(9) Uani 1 1 d . . .
N2 N 0.6041(5) 0.12229(15) 0.6894(3) 0.0523(8) Uani 1 1 d . . .
N3 N 0.0856(7) 0.2500 0.7968(4) 0.0475(10) Uani 1 2 d S . .
N4 N -0.4558(8) 0.2500 0.9009(4) 0.0604(13) Uani 1 2 d S . .
N5 N 0.3646(7) 0.2500 1.1194(4) 0.0551(12) Uani 1 2 d S . .
N6 N 0.2407(6) 0.16379(16) 0.9519(3) 0.0558(9) Uani 1 1 d . . .
C1 C 0.7383(8) 0.1191(2) 0.7961(4) 0.0745(14) Uani 1 1 d . . .
H1A H 0.6722 0.0944 0.8467 0.112 Uiso 1 1 calc R . .
H1B H 0.7558 0.1569 0.8283 0.112 Uiso 1 1 calc R . .
H1C H 0.8759 0.1038 0.7843 0.112 Uiso 1 1 calc R . .
C2 C 0.4303(7) 0.1531(2) 0.6800(4) 0.0598(11) Uani 1 1 d . . .
H2 H 0.3961 0.1743 0.7417 0.072 Uiso 1 1 calc R . .
C3 C 0.2996(7) 0.1551(2) 0.5833(4) 0.0583(11) Uani 1 1 d . . .
H3 H 0.1759 0.1774 0.5785 0.070 Uiso 1 1 calc R . .
C4 C 0.3462(6) 0.12476(17) 0.4923(3) 0.0475(9) Uani 1 1 d . . .
C5 C 0.2001(6) 0.12319(17) 0.3887(3) 0.0490(9) Uani 1 1 d . . .
C6 C 0.0235(8) 0.1563(2) 0.3729(4) 0.0642(12) Uani 1 1 d . . .
H6 H -0.0030 0.1829 0.4281 0.077 Uiso 1 1 calc R . .
C7 C -0.1141(8) 0.1517(2) 0.2796(4) 0.0693(13) Uani 1 1 d . . .
H7 H -0.2345 0.1753 0.2703 0.083 Uiso 1 1 calc R . .
C8 C -0.2408(10) 0.1077(3) 0.1046(4) 0.0856(17) Uani 1 1 d . . .
H8A H -0.1782 0.0877 0.0460 0.128 Uiso 1 1 calc R . .
H8B H -0.2899 0.1448 0.0776 0.128 Uiso 1 1 calc R . .
H8C H -0.3597 0.0859 0.1259 0.128 Uiso 1 1 calc R . .
C9 C 0.0878(9) 0.0833(2) 0.2122(4) 0.0731(14) Uani 1 1 d . . .
H9 H 0.1110 0.0576 0.1548 0.088 Uiso 1 1 calc R . .
C10 C 0.2323(8) 0.0865(2) 0.3033(4) 0.0671(12) Uani 1 1 d . . .
H10 H 0.3547 0.0636 0.3085 0.081 Uiso 1 1 calc R . .
C11 C 0.5320(7) 0.0946(2) 0.5039(4) 0.0645(12) Uani 1 1 d . . .
H11 H 0.5731 0.0742 0.4427 0.077 Uiso 1 1 calc R . .
C12 C 0.6564(8) 0.0938(2) 0.6025(4) 0.0678(12) Uani 1 1 d . . .
H12 H 0.7826 0.0724 0.6093 0.081 Uiso 1 1 calc R . .
C13 C -0.0250(8) 0.2500 0.7149(4) 0.0401(11) Uani 1 2 d S . .
C14 C -0.3009(8) 0.2500 0.9602(5) 0.0456(12) Uani 1 2 d S . .
C15 C 0.4112(8) 0.2500 1.2141(4) 0.0430(11) Uani 1 2 d S . .
C16 C 0.2491(6) 0.11586(19) 0.9500(3) 0.0487(9) Uani 1 1 d . . .
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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N6 Ni1 N6 176.9(2) 4_565 . ?
N6 Ni1 N3 89.20(10) 4_565 . ?
N6 Ni1 N3 89.20(10) . . ?
N6 Ni1 N5 90.90(10) 4_565 . ?
N6 Ni1 N5 90.90(10) . . ?
N3 Ni1 N5 175.48(18) . . ?
N6 Ni1 N4 88.74(10) 4_565 1_655 ?
N6 Ni1 N4 88.74(10) . 1_655 ?
N3 Ni1 N4 93.37(19) . 1_655 ?
N5 Ni1 N4 91.1(2) . 1_655 ?
N6 Ni1 S3 91.38(10) 4_565 . ?
N6 Ni1 S3 91.38(10) . . ?
N3 Ni1 S3 95.88(14) . . ?
N5 Ni1 S3 79.60(14) . . ?
N4 Ni1 S3 170.75(15) 1_655 . ?
C14 S3 Ni1 111.44(19) . . ?
C9 N1 C7 119.6(4) . . ?
C9 N1 C8 120.4(4) . . ?
C7 N1 C8 120.0(5) . . ?
C2 N2 C12 119.8(4) . . ?
C2 N2 C1 120.2(4) . . ?
C12 N2 C1 119.9(4) . . ?
C13 N3 Ni1 170.2(4) . . ?
C14 N4 Ni1 124.0(5) . 1_455 ?
C15 N5 Ni1 171.6(4) . . ?
C16 N6 Ni1 178.1(4) . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C2 C3 121.3(4) . . ?
N2 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C11 116.8(4) . . ?
C3 C4 C5 121.4(4) . . ?
C11 C4 C5 121.8(4) . . ?
C6 C5 C10 116.5(4) . . ?
C6 C5 C4 122.3(4) . . ?
C10 C5 C4 121.2(4) . . ?
C7 C6 C5 121.0(4) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
N1 C7 C6 121.0(5) . . ?
N1 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 122.0(4) . . ?
N1 C9 H9 119.0 . . ?
C10 C9 H9 119.0 . . ?
C9 C10 C5 119.9(5) . . ?
C9 C10 H10 120.1 . . ?
C5 C10 H10 120.1 . . ?
C12 C11 C4 120.5(4) . . ?
C12 C11 H11 119.7 . . ?
C4 C11 H11 119.7 . . ?
N2 C12 C11 121.2(4) . . ?
N2 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
N3 C13 S2 179.0(5) . . ?
N4 C14 S3 176.7(5) . . ?
N5 C15 S4 178.0(5) . . ?
N6 C16 S1 179.1(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 N6 2.045(4) 4_565 ?
Ni1 N6 2.045(4) . ?
Ni1 N3 2.058(4) . ?
Ni1 N5 2.069(5) . ?
Ni1 N4 2.154(5) 1_655 ?
Ni1 S3 2.5006(16) . ?
S1 C16 1.626(5) . ?
S2 C13 1.637(5) . ?
S3 C14 1.634(6) . ?
S4 C15 1.627(5) . ?
O1W O1W' 1.064(8) . ?
N1 C9 1.315(7) . ?
N1 C7 1.329(6) . ?
N1 C8 1.472(6) . ?
N2 C2 1.327(6) . ?
N2 C12 1.330(6) . ?
N2 C1 1.475(5) . ?
N3 C13 1.155(6) . ?
N4 C14 1.159(7) . ?
N4 Ni1 2.154(5) 1_455 ?
N5 C15 1.156(7) . ?
N6 C16 1.138(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.365(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(6) . ?
C3 H3 0.9500 . ?
C4 C11 1.383(6) . ?
C4 C5 1.482(6) . ?
C5 C6 1.374(6) . ?
C5 C10 1.388(6) . ?
C6 C7 1.360(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.363(7) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.363(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
