#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:51:50 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179458 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/55/4335551.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_4335551
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            'C38 H32 Mn N10 O4 W'
_chemical_formula_weight         931.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.1591(6)
_cell_length_b                   21.9836(12)
_cell_length_c                   36.153(2)
_cell_measurement_reflns_used    2896
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.741
_cell_measurement_theta_min      2.493
_cell_volume                     7279.4(7)
_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      130(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.922
_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  0.2589
_diffrn_reflns_av_sigmaI/netI    0.2246
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            67931
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    3.561
_exptl_absorpt_correction_T_max  0.7239
_exptl_absorpt_correction_T_min  0.1679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       plate
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.59
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.894
_refine_diff_density_min         -2.259
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.2501
_refine_ls_R_factor_gt           0.1012
_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)+(0.0000P)²+83.2247P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                3451
_reflns_number_total             8467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400845z_si_002_3.cif
_cod_data_source_block           complex3
_cod_original_cell_volume        7279.5(8)
_cod_database_code               4335551
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
W1 W 0.30049(7) 0.31525(2) 0.112465(16) 0.04099(19) Uani 1 1 d .
Mn1 Mn 0.2329(3) 0.06675(10) 0.14116(6) 0.0480(7) Uani 1 1 d .
C1 C 0.2752(15) 0.2220(5) 0.1311(4) 0.033(4) Uani 1 1 d .
C2 C 0.4086(18) 0.2564(7) 0.0747(4) 0.053(5) Uani 1 1 d .
C3 C 0.4380(17) 0.3098(8) 0.1607(5) 0.052(5) Uani 1 1 d .
C4 C 0.508(2) 0.3518(8) 0.1001(5) 0.062(5) Uani 1 1 d .
C5 C 0.275(2) 0.3666(9) 0.0626(5) 0.071(6) Uani 1 1 d .
C6 C 0.296(2) 0.4098(7) 0.1305(4) 0.058(5) Uani 1 1 d .
C7 C 0.093(2) 0.2631(7) 0.0495(6) 0.064(5) Uani 1 1 d .
H7 H 0.1809 0.2631 0.0355 0.077 Uiso 1 1 calc R
C8 C -0.028(3) 0.2447(9) 0.0327(7) 0.095(7) Uani 1 1 d .
H8 H -0.0264 0.2312 0.0078 0.115 Uiso 1 1 calc R
C9 C -0.155(3) 0.2455(10) 0.0520(7) 0.097(8) Uani 1 1 d .
H9 H -0.2433 0.2341 0.0403 0.116 Uiso 1 1 calc R
C10 C -0.155(2) 0.2628(8) 0.0886(7) 0.076(6) Uani 1 1 d .
H10 H -0.2435 0.2616 0.1025 0.091 Uiso 1 1 calc R
C11 C -0.029(2) 0.2818(7) 0.1047(6) 0.059(6) Uani 1 1 d .
C12 C -0.016(2) 0.3016(6) 0.1432(6) 0.055(5) Uani 1 1 d .
C13 C -0.132(2) 0.3000(7) 0.1667(7) 0.073(6) Uani 1 1 d .
H13 H -0.2260 0.2876 0.1584 0.088 Uiso 1 1 calc R
C14 C -0.109(3) 0.3173(9) 0.2031(6) 0.087(6) Uani 1 1 d .
H14 H -0.1864 0.3169 0.2205 0.104 Uiso 1 1 calc R
C15 C 0.027(2) 0.3349(7) 0.2135(6) 0.075(6) Uani 1 1 d .
H15 H 0.0448 0.3469 0.2383 0.090 Uiso 1 1 calc R
C16 C 0.1382(19) 0.3353(6) 0.1886(5) 0.053(5) Uani 1 1 d .
H16 H 0.2327 0.3468 0.1968 0.063 Uiso 1 1 calc R
C17 C 0.155(3) 0.0607(12) -0.0045(8) 0.141(12) Uani 1 1 d .
H17A H 0.1485 0.0162 -0.0081 0.169 Uiso 1 1 calc R
H17B H 0.1059 0.0803 -0.0259 0.169 Uiso 1 1 calc R
C18 C 0.308(3) 0.0787(10) -0.0043(5) 0.112(8) Uani 1 1 d .
H18A H 0.3145 0.1236 -0.0051 0.135 Uiso 1 1 calc R
H18B H 0.3558 0.0628 -0.0270 0.135 Uiso 1 1 calc R
C19 C 0.392(2) 0.0562(8) 0.0290(5) 0.081(6) Uani 1 1 d .
H19A H 0.4902 0.0750 0.0295 0.097 Uiso 1 1 calc R
H19B H 0.4042 0.0115 0.0276 0.097 Uiso 1 1 calc R
C20 C 0.308(2) 0.0730(8) 0.0639(4) 0.067(5) Uani 1 1 d .
H20 H 0.3061 0.1185 0.0645 0.081 Uiso 1 1 calc R
C21 C 0.499(2) 0.0263(7) 0.1024(5) 0.062(6) Uani 1 1 d .
H21 H 0.5524 0.0170 0.0805 0.074 Uiso 1 1 calc R
C22 C 0.559(2) 0.0066(7) 0.1374(5) 0.061(5) Uani 1 1 d .
C23 C 0.693(2) -0.0268(7) 0.1363(5) 0.069(5) Uani 1 1 d .
H23 H 0.7362 -0.0363 0.1131 0.083 Uiso 1 1 calc R
C24 C 0.7578(19) -0.0449(6) 0.1675(5) 0.068(6) Uani 1 1 d .
H24 H 0.8421 -0.0700 0.1661 0.081 Uiso 1 1 calc R
C25 C 0.705(2) -0.0280(7) 0.2016(6) 0.057(5) Uani 1 1 d .
C26 C 0.718(2) -0.0306(8) 0.2672(5) 0.080(6) Uani 1 1 d .
H26A H 0.7033 0.0136 0.2682 0.120 Uiso 1 1 calc R
H26B H 0.7854 -0.0429 0.2868 0.120 Uiso 1 1 calc R
H26C H 0.6237 -0.0511 0.2708 0.120 Uiso 1 1 calc R
C27 C 0.5767(18) 0.0053(6) 0.2041(5) 0.053(5) Uani 1 1 d .
H27 H 0.5386 0.0155 0.2277 0.064 Uiso 1 1 calc R
C28 C 0.503(2) 0.0240(7) 0.1722(5) 0.057(5) Uani 1 1 d .
C29 C -0.037(2) 0.1054(6) 0.1730(5) 0.052(5) Uani 1 1 d .
C30 C -0.1071(19) 0.1264(8) 0.2053(5) 0.067(5) Uani 1 1 d .
H30 H -0.0618 0.1213 0.2287 0.080 Uiso 1 1 calc R
C31 C -0.243(2) 0.1549(7) 0.2029(6) 0.063(6) Uani 1 1 d .
C32 C -0.242(2) 0.1806(9) 0.2677(5) 0.093(7) Uani 1 1 d .
H32A H -0.2283 0.1389 0.2767 0.140 Uiso 1 1 calc R
H32B H -0.3036 0.2031 0.2853 0.140 Uiso 1 1 calc R
H32C H -0.1474 0.2007 0.2655 0.140 Uiso 1 1 calc R
C33 C -0.313(2) 0.1591(8) 0.1682(7) 0.080(6) Uani 1 1 d .
H33 H -0.4073 0.1771 0.1667 0.096 Uiso 1 1 calc R
C34 C -0.251(2) 0.1388(8) 0.1375(6) 0.072(6) Uani 1 1 d .
H34 H -0.3010 0.1420 0.1146 0.086 Uiso 1 1 calc R
C35 C -0.106(2) 0.1118(7) 0.1385(5) 0.058(5) Uani 1 1 d .
C36 C -0.038(2) 0.0940(7) 0.1052(6) 0.074(6) Uani 1 1 d .
H36 H -0.0957 0.0960 0.0835 0.088 Uiso 1 1 calc R
C37 C 0.151(3) 0.0535(8) 0.0639(6) 0.089(7) Uani 1 1 d .
H37 H 0.1468 0.0080 0.0634 0.107 Uiso 1 1 calc R
C38 C 0.073(2) 0.0774(10) 0.0301(7) 0.105(8) Uani 1 1 d .
H38A H -0.0266 0.0602 0.0290 0.126 Uiso 1 1 calc R
H38B H 0.0649 0.1222 0.0318 0.126 Uiso 1 1 calc R
N1 N 0.2632(13) 0.1726(4) 0.1388(3) 0.043(4) Uani 1 1 d .
N2 N 0.4707(16) 0.2235(7) 0.0558(4) 0.075(5) Uani 1 1 d .
N3 N 0.5022(17) 0.3075(7) 0.1871(4) 0.069(4) Uani 1 1 d .
N4 N 0.6216(18) 0.3716(7) 0.0928(4) 0.085(5) Uani 1 1 d .
N5 N 0.2626(19) 0.3928(7) 0.0357(5) 0.098(6) Uani 1 1 d .
N6 N 0.2914(17) 0.4610(6) 0.1384(4) 0.067(4) Uani 1 1 d .
N7 N 0.1213(15) 0.3206(5) 0.1537(3) 0.047(3) Uani 1 1 d .
N8 N 0.0997(16) 0.2815(5) 0.0846(4) 0.054(4) Uani 1 1 d .
N9 N 0.1008(15) 0.0746(5) 0.1010(4) 0.046(3) Uiso 1 1 d .
N10 N 0.3845(16) 0.0542(7) 0.0992(4) 0.070(5) Uani 1 1 d .
O1 O 0.3832(11) 0.0578(5) 0.1758(3) 0.053(3) Uani 1 1 d .
O2 O 0.0922(11) 0.0766(4) 0.1772(3) 0.050(3) Uani 1 1 d .
O3 O 0.7762(14) -0.0470(5) 0.2323(4) 0.079(4) Uani 1 1 d .
O4 O -0.3115(14) 0.1791(6) 0.2329(4) 0.094(4) 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_1
_geom_angle_site_symmetry_3
C4 W1 C2 71.2(6) . .
C4 W1 C5 73.6(7) . .
C2 W1 C5 80.2(7) . .
C4 W1 C3 70.5(6) . .
C2 W1 C3 102.4(6) . .
C5 W1 C3 140.8(6) . .
C4 W1 C1 121.5(6) . .
C2 W1 C1 71.0(5) . .
C5 W1 C1 138.5(6) . .
C3 W1 C1 76.0(5) . .
C4 W1 C6 73.5(6) . .
C2 W1 C6 141.4(6) . .
C5 W1 C6 75.3(6) . .
C3 W1 C6 79.7(6) . .
C1 W1 C6 143.7(5) . .
C4 W1 N7 141.9(6) . .
C2 W1 N7 143.9(5) . .
C5 W1 N7 117.2(6) . .
C3 W1 N7 83.8(6) . .
C1 W1 N7 76.3(5) . .
C6 W1 N7 74.6(5) . .
C4 W1 N8 140.8(6) . .
C2 W1 N8 83.7(6) . .
C5 W1 N8 72.8(6) . .
C3 W1 N8 146.3(6) . .
C1 W1 N8 74.8(5) . .
C6 W1 N8 116.0(6) . .
N7 W1 N8 73.2(6) . .
O2 Mn1 O1 93.1(4) . .
O2 Mn1 N9 94.8(5) . .
O1 Mn1 N9 172.0(5) . .
O2 Mn1 N10 177.6(6) . .
O1 Mn1 N10 89.0(6) . .
N9 Mn1 N10 83.0(6) . .
O2 Mn1 N6 94.6(5) . 8_655
O1 Mn1 N6 89.7(5) . 8_655
N9 Mn1 N6 89.8(5) . 8_655
N10 Mn1 N6 84.2(6) . 8_655
O2 Mn1 N1 89.6(4) . .
O1 Mn1 N1 92.4(4) . .
N9 Mn1 N1 87.5(4) . .
N10 Mn1 N1 91.5(5) . .
N6 Mn1 N1 175.2(4) 8_655 .
N1 C1 W1 176.1(12) . .
N2 C2 W1 176.6(17) . .
N3 C3 W1 175.7(17) . .
N4 C4 W1 178.9(17) . .
N5 C5 W1 178.4(19) . .
N6 C6 W1 176.6(16) . .
C8 C7 N8 124(2) . .
C7 C8 C9 119(2) . .
C8 C9 C10 120(2) . .
C11 C10 C9 119(2) . .
C10 C11 N8 120(2) . .
C10 C11 C12 124.8(19) . .
N8 C11 C12 115.4(18) . .
C13 C12 N7 123.4(19) . .
C13 C12 C11 121.2(19) . .
N7 C12 C11 115.4(16) . .
C12 C13 C14 117.5(19) . .
C15 C14 C13 119(2) . .
C14 C15 C16 120(2) . .
N7 C16 C15 123.2(18) . .
C18 C17 C38 114(2) . .
C17 C18 C19 114(2) . .
C18 C19 C20 109.0(17) . .
C37 C20 N10 111.5(16) . .
C37 C20 C19 114.4(16) . .
N10 C20 C19 113.6(16) . .
N10 C21 C22 124.1(18) . .
C28 C22 C23 118.4(17) . .
C28 C22 C21 124.0(17) . .
C23 C22 C21 117.2(17) . .
C24 C23 C22 120.8(17) . .
C23 C24 C25 121.2(17) . .
O3 C25 C24 118.7(16) . .
O3 C25 C27 121.2(17) . .
C24 C25 C27 120.0(18) . .
C25 C27 C28 120.7(17) . .
O1 C28 C27 118.9(17) . .
O1 C28 C22 122.5(17) . .
C27 C28 C22 118.6(17) . .
O2 C29 C35 122.9(17) . .
O2 C29 C30 117.5(17) . .
C35 C29 C30 119.5(17) . .
C31 C30 C29 120.3(18) . .
O4 C31 C30 122.4(19) . .
O4 C31 C33 118.4(19) . .
C30 C31 C33 119(2) . .
C34 C33 C31 122(2) . .
C33 C34 C35 121(2) . .
C29 C35 C36 121.7(19) . .
C29 C35 C34 118.4(18) . .
C36 C35 C34 119.8(19) . .
N9 C36 C35 127.2(18) . .
N9 C37 C20 101.7(16) . .
N9 C37 C38 118.5(18) . .
C20 C37 C38 110.5(18) . .
C17 C38 C37 111.0(19) . .
C1 N1 Mn1 167.9(11) . .
C6 N6 Mn1 167.9(15) . 8_665
C16 N7 C12 116.5(15) . .
C16 N7 W1 124.9(12) . .
C12 N7 W1 118.3(11) . .
C7 N8 C11 117.5(16) . .
C7 N8 W1 124.8(14) . .
C11 N8 W1 117.6(13) . .
C36 N9 C37 119.4(16) . .
C36 N9 Mn1 122.7(12) . .
C37 N9 Mn1 117.7(12) . .
C21 N10 C20 128.0(16) . .
C21 N10 Mn1 124.9(14) . .
C20 N10 Mn1 105.7(11) . .
C28 O1 Mn1 127.0(11) . .
C29 O2 Mn1 126.0(10) . .
C25 O3 C26 118.0(14) . .
C31 O4 C32 121.0(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C4 2.110(19) .
W1 C2 2.127(16) .
W1 C5 2.14(2) .
W1 C3 2.155(18) .
W1 C1 2.170(11) .
W1 C6 2.179(17) .
W1 N7 2.219(12) .
W1 N8 2.224(13) .
Mn1 O2 1.844(10) .
Mn1 O1 1.870(10) .
Mn1 N9 1.899(13) .
Mn1 N10 2.076(13) .
Mn1 N6 2.337(12) 8_655
Mn1 N1 2.345(9) .
C1 N1 1.126(13) .
C2 N2 1.146(17) .
C3 N3 1.123(17) .
C4 N4 1.159(18) .
C5 N5 1.138(19) .
C6 N6 1.163(17) .
C7 C8 1.33(2) .
C7 N8 1.33(2) .
C8 C9 1.35(3) .
C9 C10 1.38(3) .
C10 C11 1.36(2) .
C11 N8 1.388(19) .
C11 C12 1.46(2) .
C12 C13 1.36(2) .
C12 N7 1.375(19) .
C13 C14 1.39(2) .
C14 C15 1.36(2) .
C15 C16 1.36(2) .
C16 N7 1.312(17) .
C17 C18 1.46(3) .
C17 C38 1.50(3) .
C18 C19 1.51(2) .
C19 C20 1.52(2) .
C20 C37 1.51(2) .
C20 N10 1.511(19) .
C21 N10 1.224(18) .
C21 C22 1.45(2) .
C22 C28 1.41(2) .
C22 C23 1.43(2) .
C23 C24 1.33(2) .
C24 C25 1.38(2) .
C25 O3 1.355(18) .
C25 C27 1.39(2) .
C26 O3 1.418(17) .
C27 C28 1.40(2) .
C28 O1 1.333(17) .
C29 O2 1.347(17) .
C29 C35 1.41(2) .
C29 C30 1.41(2) .
C30 C31 1.40(2) .
C31 O4 1.36(2) .
C31 C33 1.41(2) .
C32 O4 1.411(18) .
C33 C34 1.33(2) .
C34 C35 1.45(2) .
C35 C36 1.41(2) .
C36 N9 1.348(19) .
C37 N9 1.49(2) .
C37 C38 1.51(2) .
N6 Mn1 2.337(12) 8_665
