#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:51:50 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179458 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/55/4335549.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_4335549
loop_
_publ_author_name
'Jin Wuk Lee'
'Kwang Soo Lim'
'Dae Won Ryu'
'Eui Kwan Koh'
'Sung Won Yoon'
'Byoung Jin Suh'
'Chang Seop Hong'
_publ_section_title
;
 Cyanide-Bridged WVMnIII Bimetallic Chains Composed of a Blocked W
 Hexacyanide Precursor: Geometry-Related Magnetic Couplings and
 Magnetostructural Correlation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8677
_journal_page_last               8684
_journal_paper_doi               10.1021/ic400845z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C36 H30 Mn N10 O4 W'
_chemical_formula_weight         905.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.4420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2490(2)
_cell_length_b                   20.7220(4)
_cell_length_c                   18.0289(3)
_cell_measurement_reflns_used    8523
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.994
_cell_measurement_theta_min      2.419
_cell_volume                     3452.24(12)
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_collection       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.681
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scan'
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26620
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.60
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    3.752
_exptl_absorpt_correction_T_max  0.6896
_exptl_absorpt_correction_T_min  0.1483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       plate
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.622
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         8569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0334P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                6201
_reflns_number_total             8569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400845z_si_002_1.cif
_cod_data_source_block           complex1
_cod_database_code               4335549
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
W1 W 0.340621(19) 0.181376(8) 0.863211(7) 0.02213(6) Uani 1 1 d .
Mn1 Mn 0.22830(8) 0.44024(3) 0.77828(3) 0.03355(18) Uani 1 1 d .
C1 C 0.3138(5) 0.2838(2) 0.8394(2) 0.0300(11) Uani 1 1 d .
C2 C 0.4729(5) 0.2070(2) 0.7720(2) 0.0305(11) Uani 1 1 d .
C3 C 0.4606(5) 0.2253(2) 0.9538(2) 0.0320(11) Uani 1 1 d .
C4 C 0.5461(6) 0.1348(2) 0.8832(2) 0.0361(12) Uani 1 1 d .
C5 C 0.2956(6) 0.1044(2) 0.9384(2) 0.0422(13) Uani 1 1 d .
C6 C 0.3423(5) 0.0928(2) 0.7995(2) 0.0317(11) Uani 1 1 d .
C7 C 0.1598(5) 0.2249(2) 1.0022(2) 0.0402(13) Uani 1 1 d .
H7 H 0.2499 0.2237 1.0271 0.048 Uiso 1 1 calc R
C8 C 0.0397(6) 0.2401(3) 1.0419(3) 0.0491(15) Uani 1 1 d .
H8 H 0.0491 0.2502 1.0922 0.059 Uiso 1 1 calc R
C9 C -0.0929(6) 0.2400(3) 1.0056(3) 0.0511(15) Uani 1 1 d .
H9 H -0.1758 0.2488 1.0311 0.061 Uiso 1 1 calc R
C10 C -0.1026(5) 0.2267(3) 0.9309(3) 0.0453(14) Uani 1 1 d .
H10 H -0.1923 0.2270 0.9055 0.054 Uiso 1 1 calc R
C11 C 0.0214(5) 0.2128(2) 0.8936(2) 0.0292(10) Uani 1 1 d .
C12 C 0.0193(5) 0.2001(2) 0.8139(2) 0.0307(11) Uani 1 1 d .
C13 C -0.1036(6) 0.2031(3) 0.7687(3) 0.0464(14) Uani 1 1 d .
H13 H -0.1930 0.2104 0.7888 0.056 Uiso 1 1 calc R
C14 C -0.0936(7) 0.1950(3) 0.6931(3) 0.0522(16) Uani 1 1 d .
H14 H -0.1764 0.1968 0.6621 0.063 Uiso 1 1 calc R
C15 C 0.0388(6) 0.1844(2) 0.6640(2) 0.0452(14) Uani 1 1 d .
H15 H 0.0474 0.1799 0.6130 0.054 Uiso 1 1 calc R
C16 C 0.1577(6) 0.1805(2) 0.7113(2) 0.0370(12) Uani 1 1 d .
H16 H 0.2474 0.1728 0.6916 0.044 Uiso 1 1 calc R
C17 C 0.2826(7) 0.4056(3) 0.6303(3) 0.071(2) Uani 1 1 d .
H17A H 0.3148 0.4230 0.5838 0.085 Uiso 1 1 calc R
H17B H 0.3108 0.3606 0.6329 0.085 Uiso 1 1 calc R
C18 C 0.1248(7) 0.4102(3) 0.6311(3) 0.070(2) Uani 1 1 d .
H18A H 0.0814 0.3756 0.6014 0.084 Uiso 1 1 calc R
H18B H 0.0931 0.4510 0.6097 0.084 Uiso 1 1 calc R
C19 C -0.0530(7) 0.3869(2) 0.7228(2) 0.0433(14) Uani 1 1 d .
C20 C -0.1556(7) 0.3662(3) 0.6588(3) 0.075(2) Uani 1 1 d .
H20A H -0.1611 0.3996 0.6219 0.112 Uiso 1 1 calc R
H20B H -0.2501 0.3586 0.6770 0.112 Uiso 1 1 calc R
H20C H -0.1202 0.3273 0.6371 0.112 Uiso 1 1 calc R
C21 C -0.1070(6) 0.3868(2) 0.7974(2) 0.0361(12) Uani 1 1 d .
C22 C -0.2450(6) 0.3615(3) 0.8129(3) 0.0490(14) Uani 1 1 d .
H22 H -0.3005 0.3430 0.7743 0.059 Uiso 1 1 calc R
C23 C -0.2996(6) 0.3632(3) 0.8815(3) 0.0515(15) Uani 1 1 d .
H23 H -0.3907 0.3460 0.8892 0.062 Uiso 1 1 calc R
C24 C -0.2185(6) 0.3909(2) 0.9407(3) 0.0404(13) Uani 1 1 d .
C25 C -0.1973(6) 0.4180(3) 1.0691(3) 0.0570(16) Uani 1 1 d .
H25A H -0.1126 0.3922 1.0793 0.085 Uiso 1 1 calc R
H25B H -0.2550 0.4189 1.1121 0.085 Uiso 1 1 calc R
H25C H -0.1689 0.4612 1.0570 0.085 Uiso 1 1 calc R
C26 C -0.0852(5) 0.4171(2) 0.9285(2) 0.0344(11) Uani 1 1 d .
H26 H -0.0319 0.4358 0.9678 0.041 Uiso 1 1 calc R
C27 C -0.0287(5) 0.4161(2) 0.8581(2) 0.0305(11) Uani 1 1 d .
C28 C 0.4981(5) 0.5012(2) 0.8228(2) 0.0335(12) Uani 1 1 d .
C29 C 0.5757(5) 0.5310(2) 0.8821(2) 0.0381(12) Uani 1 1 d .
H29 H 0.5369 0.5317 0.9289 0.046 Uiso 1 1 calc R
C30 C 0.7082(6) 0.5590(2) 0.8721(3) 0.0435(13) Uani 1 1 d .
C31 C 0.7194(6) 0.6010(3) 0.9956(3) 0.0629(17) Uani 1 1 d .
H31A H 0.6274 0.6218 0.9871 0.094 Uiso 1 1 calc R
H31B H 0.7808 0.6278 1.0270 0.094 Uiso 1 1 calc R
H31C H 0.7055 0.5601 1.0193 0.094 Uiso 1 1 calc R
C32 C 0.7664(6) 0.5574(3) 0.8027(3) 0.0556(16) Uani 1 1 d .
H32 H 0.8582 0.5743 0.7961 0.067 Uiso 1 1 calc R
C33 C 0.6895(6) 0.5310(3) 0.7438(3) 0.0501(15) Uani 1 1 d .
H33 H 0.7294 0.5322 0.6973 0.060 Uiso 1 1 calc R
C34 C 0.5522(5) 0.5019(2) 0.7500(2) 0.0371(12) Uani 1 1 d .
C35 C 0.4769(6) 0.4719(2) 0.6868(2) 0.0421(14) Uani 1 1 d .
C36 C 0.5401(7) 0.4780(3) 0.6108(3) 0.078(2) Uani 1 1 d .
H36A H 0.5673 0.4360 0.5936 0.117 Uiso 1 1 calc R
H36B H 0.6239 0.5054 0.6141 0.117 Uiso 1 1 calc R
H36C H 0.4691 0.4964 0.5766 0.117 Uiso 1 1 calc R
N1 N 0.2907(5) 0.3351(2) 0.8204(2) 0.0446(11) Uani 1 1 d .
N2 N 0.5423(5) 0.2218(2) 0.7242(2) 0.0492(12) Uani 1 1 d .
N3 N 0.5245(5) 0.2476(2) 1.0026(2) 0.0531(13) Uani 1 1 d .
N4 N 0.6571(5) 0.1105(2) 0.8942(2) 0.0573(13) Uani 1 1 d .
N5 N 0.2671(6) 0.0650(2) 0.9791(2) 0.0708(17) Uani 1 1 d .
N6 N 0.3368(5) 0.0472(2) 0.7652(2) 0.0425(11) Uani 1 1 d .
N7 N 0.1518(4) 0.21180(18) 0.92901(17) 0.0281(9) Uani 1 1 d .
N8 N 0.1504(4) 0.18727(16) 0.78585(17) 0.0285(9) Uani 1 1 d .
N9 N 0.0774(5) 0.40532(19) 0.70864(18) 0.0401(11) Uani 1 1 d .
N10 N 0.3552(5) 0.44102(19) 0.69280(19) 0.0418(11) Uani 1 1 d .
O1 O 0.0971(3) 0.44520(15) 0.85252(14) 0.0353(8) Uani 1 1 d .
O2 O 0.3747(3) 0.47394(15) 0.83949(15) 0.0366(8) Uani 1 1 d .
O3 O -0.2806(4) 0.39067(18) 1.0075(2) 0.0553(10) Uani 1 1 d .
O4 O 0.7852(4) 0.59118(19) 0.9265(2) 0.0582(11) 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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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_3
C3 W1 C5 86.70(18) .
C3 W1 C4 68.71(17) .
C5 W1 C4 75.77(18) .
C3 W1 C2 100.63(17) .
C5 W1 C2 142.76(18) .
C4 W1 C2 73.25(17) .
C3 W1 C6 138.66(17) .
C5 W1 C6 73.18(17) .
C4 W1 C6 71.45(17) .
C2 W1 C6 77.74(16) .
C3 W1 C1 77.68(17) .
C5 W1 C1 145.66(16) .
C4 W1 C1 124.30(18) .
C2 W1 C1 70.93(16) .
C6 W1 C1 136.47(15) .
C3 W1 N8 146.60(15) .
C5 W1 N8 105.67(17) .
C4 W1 N8 143.95(15) .
C2 W1 N8 88.14(15) .
C6 W1 N8 74.60(15) .
C1 W1 N8 74.92(15) .
C3 W1 N7 82.33(15) .
C5 W1 N7 72.47(15) .
C4 W1 N7 137.82(14) .
C2 W1 N7 144.43(16) .
C6 W1 N7 122.82(16) .
C1 W1 N7 75.24(14) .
N8 W1 N7 72.56(13) .
O2 Mn1 O1 91.91(13) .
O2 Mn1 N9 177.21(15) .
O1 Mn1 N9 90.73(15) .
O2 Mn1 N10 91.06(16) .
O1 Mn1 N10 174.04(16) .
N9 Mn1 N10 86.23(17) .
O2 Mn1 N1 89.66(15) .
O1 Mn1 N1 88.72(14) .
N9 Mn1 N1 91.29(16) .
N10 Mn1 N1 96.47(15) .
O2 Mn1 N6 90.75(14) 2_556
O1 Mn1 N6 91.25(14) 2_556
N9 Mn1 N6 88.30(15) 2_556
N10 Mn1 N6 83.54(15) 2_556
N1 Mn1 N6 179.59(15) 2_556
N1 C1 W1 172.4(4) .
N2 C2 W1 178.7(4) .
N3 C3 W1 178.8(5) .
N4 C4 W1 179.2(5) .
N5 C5 W1 177.2(5) .
N6 C6 W1 176.8(4) .
N7 C7 C8 122.8(5) .
C9 C8 C7 118.4(4) .
C8 C9 C10 119.4(5) .
C9 C10 C11 119.8(5) .
N7 C11 C10 121.3(4) .
N7 C11 C12 116.1(4) .
C10 C11 C12 122.6(4) .
N8 C12 C13 121.1(4) .
N8 C12 C11 115.2(4) .
C13 C12 C11 123.6(4) .
C12 C13 C14 119.6(5) .
C15 C14 C13 119.8(5) .
C16 C15 C14 118.6(5) .
N8 C16 C15 122.7(5) .
C18 C17 N10 112.4(4) .
C17 C18 N9 109.8(5) .
N9 C19 C21 122.6(4) .
N9 C19 C20 119.2(5) .
C21 C19 C20 118.2(5) .
C22 C21 C27 116.0(4) .
C22 C21 C19 122.0(5) .
C27 C21 C19 121.8(5) .
C23 C22 C21 123.0(5) .
C22 C23 C24 119.8(5) .
O3 C24 C26 124.1(5) .
O3 C24 C23 116.2(5) .
C26 C24 C23 119.6(4) .
C24 C26 C27 121.0(4) .
O1 C27 C26 115.5(4) .
O1 C27 C21 124.0(4) .
C26 C27 C21 120.6(4) .
O2 C28 C29 115.6(4) .
O2 C28 C34 123.7(4) .
C29 C28 C34 120.6(4) .
C30 C29 C28 120.9(4) .
O4 C30 C29 123.6(5) .
O4 C30 C32 116.9(5) .
C29 C30 C32 119.5(5) .
C33 C32 C30 120.2(5) .
C32 C33 C34 123.3(5) .
C33 C34 C28 115.4(5) .
C33 C34 C35 121.5(4) .
C28 C34 C35 123.0(4) .
N10 C35 C34 122.2(4) .
N10 C35 C36 118.9(5) .
C34 C35 C36 119.0(5) .
C1 N1 Mn1 176.6(4) .
C6 N6 Mn1 161.6(4) 2_546
C11 N7 C7 118.3(4) .
C11 N7 W1 117.2(3) .
C7 N7 W1 124.3(3) .
C16 N8 C12 118.2(4) .
C16 N8 W1 123.4(3) .
C12 N8 W1 118.5(3) .
C19 N9 C18 121.1(4) .
C19 N9 Mn1 128.3(3) .
C18 N9 Mn1 110.2(3) .
C35 N10 C17 123.0(4) .
C35 N10 Mn1 127.8(3) .
C17 N10 Mn1 108.9(3) .
C27 O1 Mn1 129.7(3) .
C28 O2 Mn1 130.1(3) .
C24 O3 C25 116.8(4) .
C30 O4 C31 118.0(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C3 2.139(4) .
W1 C5 2.146(5) .
W1 C4 2.148(5) .
W1 C2 2.157(4) .
W1 C6 2.164(5) .
W1 C1 2.177(5) .
W1 N8 2.202(4) .
W1 N7 2.243(3) .
Mn1 O2 1.847(3) .
Mn1 O1 1.847(3) .
Mn1 N9 1.975(4) .
Mn1 N10 1.976(4) .
Mn1 N1 2.370(4) .
Mn1 N6 2.419(4) 2_556
C1 N1 1.135(6) .
C2 N2 1.138(5) .
C3 N3 1.137(5) .
C4 N4 1.153(6) .
C5 N5 1.136(5) .
C6 N6 1.130(5) .
C7 N7 1.346(5) .
C7 C8 1.383(6) .
C8 C9 1.366(7) .
C9 C10 1.373(6) .
C10 C11 1.385(6) .
C11 N7 1.340(5) .
C11 C12 1.460(5) .
C12 N8 1.360(5) .
C12 C13 1.372(6) .
C13 C14 1.379(7) .
C14 C15 1.370(7) .
C15 C16 1.365(6) .
C16 N8 1.356(5) .
C17 C18 1.463(8) .
C17 N10 1.481(6) .
C18 N9 1.486(5) .
C19 N9 1.301(6) .
C19 C21 1.455(6) .
C19 C20 1.523(6) .
C21 C22 1.418(7) .
C21 C27 1.423(6) .
C22 C23 1.355(6) .
C23 C24 1.402(7) .
C24 O3 1.356(5) .
C24 C26 1.374(6) .
C25 O3 1.441(6) .
C26 C27 1.393(6) .
C27 O1 1.318(5) .
C28 O2 1.320(5) .
C28 C29 1.405(6) .
C28 C34 1.424(5) .
C29 C30 1.376(6) .
C30 O4 1.362(6) .
C30 C32 1.383(6) .
C31 O4 1.425(6) .
C32 C33 1.367(7) .
C33 C34 1.415(7) .
C34 C35 1.449(7) .
C35 N10 1.304(6) .
C35 C36 1.517(6) .
N6 Mn1 2.419(4) 2_546
