#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:27:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179481 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/78/4337889.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_4337889
loop_
_publ_author_name
'Stefańczyk, Olaf'
'Rams, Michał'
'Majcher, Anna M.'
'Mathonière, Corine'
'Sieklucka, Barbara'
_publ_section_title
;
 Chiral (LH)2L2Cu3 Trinuclear Paramagnetic Nodes in
 Octacyanidometalate-Bridged Helical Chains.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3874
_journal_paper_doi               10.1021/ic500271f
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C20 H38 Cu3 N16 O4 W, H2 O'
_chemical_formula_sum            'C20 H40 Cu3 N16 O5 W'
_chemical_formula_weight         959.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_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_date             2013-10-17T15:14:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2460(2)
_cell_length_b                   17.5290(2)
_cell_length_c                   20.6140(4)
_cell_measurement_reflns_used    7741
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6231.72(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.325765E-1
_diffrn_orient_matrix_UB_12      -0.437782E-1
_diffrn_orient_matrix_UB_13      0.149882E-1
_diffrn_orient_matrix_UB_21      -0.35648E-1
_diffrn_orient_matrix_UB_22      -0.78382E-2
_diffrn_orient_matrix_UB_23      0.37676E-1
_diffrn_orient_matrix_UB_31      -0.320972E-1
_diffrn_orient_matrix_UB_32      -0.357266E-1
_diffrn_orient_matrix_UB_33      -0.266319E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13556
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.77
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.760
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.329
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.78
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0351P)²+8.4796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                6563
_reflns_number_total             7101
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic500271f_si_003.cif
_cod_data_source_block           CubdapW
_cod_depositor_comments
'Adding full bibliography for 4337888--4337889.cif.'
_cod_database_code               4337889
#BEGIN Tags that were not found in dictionaries:
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, 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
W1 W 0.655949(6) 0.727491(6) 0.135504(5) 0.01017(4) Uani 1 1 d .
Cu1 Cu 0.374362(19) 0.637034(18) 0.197494(16) 0.01518(7) Uani 1 1 d .
Cu3 Cu 0.806108(19) 0.962123(19) 0.022475(15) 0.01600(7) Uani 1 1 d .
Cu2 Cu 0.713247(19) 0.868581(18) -0.087215(16) 0.01718(8) Uani 1 1 d .
N6 N 0.64765(14) 0.62057(16) 0.00341(13) 0.0228(5) Uani 1 1 d .
C3 C 0.59298(15) 0.75405(16) 0.22452(13) 0.0155(5) Uani 1 1 d .
C8 C 0.68029(16) 0.63293(15) 0.19995(13) 0.0162(5) Uani 1 1 d .
O5 O 0.49957(15) 0.84037(15) 0.93824(13) 0.0315(5) Uani 1 1 d .
N8 N 0.68926(15) 0.58253(15) 0.23506(13) 0.0257(5) Uani 1 1 d .
C6 C 0.65044(14) 0.65780(16) 0.04939(13) 0.0154(5) Uani 1 1 d .
C24 C 0.7291(2) 0.72175(17) -0.14062(16) 0.0243(7) Uani 1 1 d .
C44 C 0.93273(17) 0.84650(16) 0.01730(14) 0.0200(5) Uani 1 1 d .
N1 N 0.49212(14) 0.62753(14) 0.14175(11) 0.0191(5) Uani 1 1 d .
C5 C 0.57139(16) 0.80887(16) 0.10028(13) 0.0179(5) Uani 1 1 d .
O1 O 0.34582(13) 0.47953(14) 0.31475(11) 0.0265(5) Uani 1 1 d .
C7 C 0.72170(15) 0.81098(15) 0.18802(13) 0.0162(5) Uani 1 1 d .
N2 N 0.73106(15) 0.83572(14) 0.01967(12) 0.0229(5) Uani 1 1 d .
C22 C 0.3738(2) 0.78966(19) 0.1560(2) 0.0337(8) Uani 1 1 d .
O4 O 1.01965(13) 0.93829(12) 0.06642(10) 0.0202(4) Uani 1 1 d .
C4 C 0.77606(16) 0.69502(15) 0.11997(13) 0.0158(5) Uani 1 1 d .
C2 C 0.70491(15) 0.79918(15) 0.06063(12) 0.0145(5) Uani 1 1 d .
C12 C 0.46633(19) 0.53421(19) 0.28810(16) 0.0280(6) Uani 1 1 d .
N41 N 0.86602(16) 0.97016(16) 0.10699(12) 0.0234(5) Uani 1 1 d .
N7 N 0.75788(15) 0.85668(15) 0.21468(12) 0.0235(5) Uani 1 1 d .
N5 N 0.52859(15) 0.85218(16) 0.07855(14) 0.0293(6) Uani 1 1 d .
N4 N 0.83987(14) 0.68000(14) 0.10923(13) 0.0223(5) Uani 1 1 d .
N15 N 0.33318(14) 0.53182(14) 0.18706(12) 0.0172(5) Uani 1 1 d .
N45 N 0.89524(14) 0.90932(14) -0.01931(11) 0.0164(4) Uani 1 1 d .
C33 C 0.69011(16) 1.02142(16) -0.05975(14) 0.0188(5) Uani 1 1 d .
O3 O 0.75345(10) 0.96926(10) -0.06336(9) 0.0151(4) Uani 1 1 d .
O2 O 0.31365(11) 0.67237(11) 0.12149(10) 0.0180(4) Uani 1 1 d .
N35 N 0.71007(15) 1.01305(16) 0.05590(12) 0.0212(5) Uani 1 1 d .
C14 C 0.38460(18) 0.46716(16) 0.20254(14) 0.0206(5) Uani 1 1 d .
N25 N 0.66914(16) 0.76512(14) -0.10425(13) 0.0196(5) Uani 1 1 d .
C43 C 0.96873(16) 0.87551(16) 0.07983(13) 0.0191(5) Uani 1 1 d .
N31 N 0.62252(15) 0.92460(15) -0.12316(14) 0.0205(5) Uani 1 1 d .
N21 N 0.38401(17) 0.74865(16) 0.21788(16) 0.0279(6) Uani 1 1 d .
C42 C 0.90936(18) 0.9020(2) 0.12918(14) 0.0238(6) Uani 1 1 d .
N11 N 0.43098(16) 0.60992(16) 0.28042(12) 0.0230(5) Uani 1 1 d .
C34 C 0.64908(16) 1.01033(18) 0.00529(15) 0.0211(6) Uani 1 1 d .
C32 C 0.63604(18) 1.00773(16) -0.11731(15) 0.0209(5) Uani 1 1 d .
C13 C 0.41086(18) 0.46980(17) 0.27303(14) 0.0222(6) Uani 1 1 d .
C23 C 0.30858(19) 0.75357(16) 0.11729(16) 0.0244(6) Uani 1 1 d .
H23 H 0.3144 0.7688 0.0708 0.029 Uiso 1 1 calc R
N3 N 0.55776(15) 0.76380(15) 0.27177(12) 0.0231(5) Uani 1 1 d .
C1 C 0.54886(16) 0.66157(16) 0.13735(12) 0.0146(5) Uani 1 1 d .
H43 H 0.9992(18) 0.8314(18) 0.0991(15) 0.013(7) Uiso 1 1 d .
H32A H 0.659(2) 1.024(2) -0.155(2) 0.024(9) Uiso 1 1 d .
H45B H 0.926(2) 0.940(2) -0.0291(17) 0.021(9) Uiso 1 1 d .
H34B H 0.6245(19) 0.9584(18) 0.0086(16) 0.013(7) Uiso 1 1 d .
H15B H 0.293(2) 0.531(2) 0.2138(18) 0.021(8) Uiso 1 1 d .
H14B H 0.356(2) 0.417(2) 0.1948(18) 0.023(9) Uiso 1 1 d .
H13 H 0.445(2) 0.421(2) 0.279(2) 0.039(11) Uiso 1 1 d .
H44B H 0.979(2) 0.819(2) -0.0096(18) 0.027(9) Uiso 1 1 d .
H414 H 0.726(2) 0.739(2) -0.188(2) 0.029(10) Uiso 1 1 d .
H35A H 0.725(2) 1.062(3) 0.063(2) 0.036(11) Uiso 1 1 d .
H34A H 0.608(2) 1.050(2) 0.0128(17) 0.023(9) Uiso 1 1 d .
H406 H 0.657(2) 0.743(2) -0.066(2) 0.030(10) Uiso 1 1 d .
H404 H 0.718(2) 0.666(2) -0.1340(17) 0.027(10) Uiso 1 1 d .
H42A H 0.874(2) 0.860(2) 0.1375(16) 0.021(9) Uiso 1 1 d .
H4 H 1.053(2) 0.921(2) 0.0524(19) 0.023(10) Uiso 1 1 d .
H35B H 0.695(2) 0.994(2) 0.089(2) 0.023(9) Uiso 1 1 d .
H44A H 0.891(2) 0.813(2) 0.0281(18) 0.026(9) Uiso 1 1 d .
H42B H 0.934(3) 0.913(2) 0.170(2) 0.043(11) Uiso 1 1 d .
H32B H 0.590(2) 1.039(2) -0.1102(18) 0.024(9) Uiso 1 1 d .
H416 H 0.623(3) 0.768(2) -0.127(2) 0.031(11) Uiso 1 1 d .
H33 H 0.714(2) 1.077(2) -0.0607(18) 0.027(9) Uiso 1 1 d .
H12A H 0.513(2) 0.531(2) 0.2596(18) 0.026(9) Uiso 1 1 d .
H14A H 0.426(3) 0.469(2) 0.174(2) 0.038(11) Uiso 1 1 d .
H45A H 0.874(2) 0.888(2) -0.055(2) 0.029(9) Uiso 1 1 d .
H31A H 0.621(2) 0.913(2) -0.163(2) 0.024(9) Uiso 1 1 d .
H15A H 0.312(3) 0.527(3) 0.145(2) 0.040(11) Uiso 1 1 d .
H11B H 0.399(2) 0.615(2) 0.312(2) 0.032(10) Uiso 1 1 d .
H31B H 0.583(3) 0.912(2) -0.105(2) 0.036(11) Uiso 1 1 d .
H41B H 0.901(3) 1.005(3) 0.098(3) 0.071(17) Uiso 1 1 d .
H304 H 0.314(3) 0.441(3) 0.301(2) 0.043(12) Uiso 1 1 d .
H41A H 0.833(3) 0.986(3) 0.136(2) 0.038(12) Uiso 1 1 d .
H22A H 0.424(3) 0.786(3) 0.133(2) 0.052(14) Uiso 1 1 d .
H12B H 0.482(2) 0.528(2) 0.336(2) 0.039(11) Uiso 1 1 d .
H22B H 0.365(3) 0.841(3) 0.165(2) 0.054(13) Uiso 1 1 d .
H21A H 0.430(3) 0.752(2) 0.235(2) 0.035(11) Uiso 1 1 d .
H11A H 0.465(3) 0.643(3) 0.283(2) 0.042(12) Uiso 1 1 d .
H21B H 0.352(3) 0.762(3) 0.240(3) 0.056(17) Uiso 1 1 d .
H5B H 0.501(3) 0.842(3) 0.976(2) 0.041(12) Uiso 1 1 d .
H5A H 0.455(4) 0.836(3) 0.928(3) 0.072(18) Uiso 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.849 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
C7 W1 C6 145.61(10) . .
C7 W1 C2 75.95(10) . .
C6 W1 C2 76.05(10) . .
C7 W1 C5 94.35(10) . .
C6 W1 C5 93.87(10) . .
C2 W1 C5 68.94(10) . .
C7 W1 C8 96.33(10) . .
C6 W1 C8 94.58(10) . .
C2 W1 C8 143.82(10) . .
C5 W1 C8 147.20(10) . .
C7 W1 C4 75.46(10) . .
C6 W1 C4 76.83(10) . .
C2 W1 C4 71.01(10) . .
C5 W1 C4 139.95(10) . .
C8 W1 C4 72.84(10) . .
C7 W1 C1 143.25(9) . .
C6 W1 C1 71.14(9) . .
C2 W1 C1 130.67(9) . .
C5 W1 C1 77.55(10) . .
C8 W1 C1 75.38(10) . .
C4 W1 C1 132.22(10) . .
C7 W1 C3 72.13(10) . .
C6 W1 C3 142.27(10) . .
C2 W1 C3 132.11(10) . .
C5 W1 C3 78.83(10) . .
C8 W1 C3 75.16(10) . .
C4 W1 C3 130.87(10) . .
C1 W1 C3 71.14(10) . .
O2 Cu1 N15 90.90(9) . .
O2 Cu1 N21 84.53(11) . .
N15 Cu1 N21 162.97(11) . .
O2 Cu1 N11 173.97(10) . .
N15 Cu1 N11 92.63(11) . .
N21 Cu1 N11 90.69(12) . .
O2 Cu1 N1 95.31(8) . .
N15 Cu1 N1 101.01(10) . .
N21 Cu1 N1 95.76(11) . .
N11 Cu1 N1 88.82(10) . .
N45 Cu3 O3 89.82(9) . .
N45 Cu3 N35 173.92(10) . .
O3 Cu3 N35 84.30(9) . .
N45 Cu3 N41 90.61(10) . .
O3 Cu3 N41 171.66(10) . .
N35 Cu3 N41 95.43(11) . .
O3 Cu2 N31 85.83(9) . .
O3 Cu2 N25 175.40(10) . .
N31 Cu2 N25 94.77(11) . .
O3 Cu2 O2 96.05(8) . 3_565
N31 Cu2 O2 136.47(10) . 3_565
N25 Cu2 O2 86.66(10) . 3_565
O3 Cu2 N2 86.44(8) . .
N31 Cu2 N2 125.85(11) . .
N25 Cu2 N2 89.53(10) . .
O2 Cu2 N2 97.63(9) 3_565 .
N3 C3 W1 175.9(2) . .
N8 C8 W1 176.5(2) . .
N6 C6 W1 179.9(3) . .
N25 C24 C23 108.9(2) . 3_565
N45 C44 C43 111.2(2) . .
C1 N1 Cu1 137.8(2) . .
N5 C5 W1 176.4(2) . .
N7 C7 W1 178.1(2) . .
C2 N2 Cu2 142.2(2) . .
N21 C22 C23 109.9(3) . .
N4 C4 W1 176.8(2) . .
N2 C2 W1 178.2(2) . .
N11 C12 C13 113.0(3) . .
C42 N41 Cu3 117.77(19) . .
C14 N15 Cu1 118.36(18) . .
C44 N45 Cu3 117.50(18) . .
O3 C33 C32 109.0(2) . .
O3 C33 C34 108.6(2) . .
C32 C33 C34 112.2(2) . .
C33 O3 Cu2 108.63(16) . .
C33 O3 Cu3 110.05(16) . .
Cu2 O3 Cu3 109.13(9) . .
C23 O2 Cu1 113.04(18) . .
C23 O2 Cu2 106.42(17) . 3_465
Cu1 O2 Cu2 128.53(10) . 3_465
C34 N35 Cu3 109.28(17) . .
N15 C14 C13 111.2(2) . .
C24 N25 Cu2 106.74(18) . .
O4 C43 C42 107.9(2) . .
O4 C43 C44 110.1(2) . .
C42 C43 C44 113.3(2) . .
C32 N31 Cu2 109.36(18) . .
C22 N21 Cu1 106.5(2) . .
N41 C42 C43 112.4(2) . .
C12 N11 Cu1 120.2(2) . .
N35 C34 C33 106.5(2) . .
N31 C32 C33 108.3(2) . .
O1 C13 C12 106.6(2) . .
O1 C13 C14 110.2(2) . .
C12 C13 C14 114.0(3) . .
O2 C23 C24 108.7(2) . 3_465
O2 C23 C22 109.8(3) . .
C24 C23 C22 112.6(3) 3_465 .
N1 C1 W1 176.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C7 2.145(3) .
W1 C6 2.157(3) .
W1 C2 2.162(3) .
W1 C5 2.165(3) .
W1 C8 2.165(3) .
W1 C4 2.172(3) .
W1 C1 2.179(3) .
W1 C3 2.183(3) .
Cu1 O2 1.984(2) .
Cu1 N15 1.988(2) .
Cu1 N21 2.008(3) .
Cu1 N11 2.025(3) .
Cu1 N1 2.339(2) .
Cu3 N45 1.990(2) .
Cu3 O3 1.9928(19) .
Cu3 N35 2.004(3) .
Cu3 N41 2.030(3) .
Cu2 O3 1.9588(18) .
Cu2 N31 1.990(3) .
Cu2 N25 1.998(2) .
Cu2 O2 2.003(2) 3_565
Cu2 N2 2.298(3) .
N6 C6 1.152(4) .
C3 N3 1.160(4) .
C8 N8 1.153(4) .
C24 N25 1.486(4) .
C24 C23 1.516(4) 3_565
C44 N45 1.483(4) .
C44 C43 1.518(4) .
N1 C1 1.150(4) .
C5 N5 1.150(4) .
O1 C13 1.424(4) .
C7 N7 1.155(4) .
N2 C2 1.152(4) .
C22 N21 1.475(5) .
C22 C23 1.517(5) .
O4 C43 1.435(3) .
C4 N4 1.153(4) .
C12 N11 1.469(4) .
C12 C13 1.512(4) .
N41 C42 1.481(4) .
N15 C14 1.474(4) .
C33 O3 1.426(3) .
C33 C32 1.528(4) .
C33 C34 1.528(4) .
O2 C23 1.429(3) .
O2 Cu2 2.003(2) 3_465
N35 C34 1.482(4) .
C14 C13 1.523(4) .
C43 C42 1.516(4) .
N31 C32 1.481(4) .
C23 C24 1.516(4) 3_465
