#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/18/4311870.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_4311870
loop_
_publ_author_name
'Young Sin You'
'Dohyeon Kim'
'Youngkyu Do'
'Sang Jun Oh'
'Chang Seop Hong'
_publ_section_title
;
 One-Dimensional Octacyanomolybdate-Based Cu(II)-Mo(V) Bimetallic Assembly
 with a Novel Rope-Ladder Chain Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6899
_journal_page_last               6901
_journal_paper_doi               10.1021/ic048856i
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C23 H41 Cu1.5 Mo N14 O2.5'
_chemical_formula_weight         744.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.32(4)
_cell_angle_beta                 83.15(3)
_cell_angle_gamma                69.71(3)
_cell_formula_units_Z            2
_cell_length_a                   8.904(3)
_cell_length_b                   10.056(4)
_cell_length_c                   19.464(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1598.5(12)
_computing_structure_refinement  WinGX
_computing_structure_solution    WinGX
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18379
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    1.428
_exptl_crystal_colour            pink-brown
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             765
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0420
_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)+(0.0560P)²+1.5499P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                5813
_reflns_number_total             7212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048856isi20040818_101209.cif
_cod_data_source_block           complex1
_cod_original_formula_sum        'C23 H41 Cu1.50 Mo N14 O2.50'
_cod_database_code               4311870
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Mo1 Mo 0.17713(3) 0.10261(3) 0.249208(14) 0.02802(9) Uani 1 1 d . . .
C1 C 0.3463(4) 0.0588(4) 0.32810(18) 0.0350(8) Uani 1 1 d . . .
N1 N 0.4276(4) 0.0363(4) 0.37269(19) 0.0523(9) Uani 1 1 d . . .
C2 C 0.1885(4) -0.1051(4) 0.30992(19) 0.0364(8) Uani 1 1 d . . .
N2 N 0.1956(4) -0.2143(4) 0.34303(19) 0.0524(9) Uani 1 1 d . . .
C3 C 0.0149(5) 0.2851(4) 0.18424(19) 0.0412(9) Uani 1 1 d . . .
N3 N -0.0723(5) 0.3828(4) 0.15140(17) 0.0542(10) Uani 1 1 d . . .
C4 C -0.0621(5) 0.1053(5) 0.2864(2) 0.0588(13) Uani 1 1 d . . .
N4 N -0.1872(5) 0.1043(6) 0.3064(3) 0.0959(18) Uani 1 1 d . . .
C5 C 0.3963(4) -0.0431(4) 0.2082(2) 0.0370(8) Uani 1 1 d . . .
N5 N 0.5092(4) -0.1205(4) 0.1853(2) 0.0502(9) Uani 1 1 d . . .
C6 C 0.1173(6) 0.0189(4) 0.1675(2) 0.0482(10) Uani 1 1 d . . .
N6 N 0.0857(8) -0.0237(5) 0.1235(3) 0.0949(18) Uani 1 1 d . . .
C7 C 0.0910(6) 0.2659(5) 0.3143(2) 0.0602(13) Uani 1 1 d . . .
N7 N 0.0414(7) 0.3528(5) 0.3490(3) 0.101(2) Uani 1 1 d . . .
C8 C 0.3161(6) 0.2329(4) 0.1955(2) 0.0505(10) Uani 1 1 d . . .
N8 N 0.3952(7) 0.2965(5) 0.1657(3) 0.0842(15) Uani 1 1 d . . .
Cu1 Cu 0.71416(5) -0.35088(5) 0.15775(2) 0.03702(12) Uani 1 1 d . . .
N9 N 0.8932(4) -0.2674(4) 0.14593(17) 0.0425(7) Uani 1 1 d . . .
C9 C 1.0086(5) -0.3024(6) 0.0848(3) 0.0599(12) Uani 1 1 d . . .
H9A H 1.0604 -0.4059 0.0903 0.072 Uiso 1 1 calc R . .
H9B H 1.0908 -0.2591 0.0839 0.072 Uiso 1 1 calc R . .
C10 C 0.9272(7) -0.2491(6) 0.0170(3) 0.0690(14) Uani 1 1 d . . .
H10A H 1.0088 -0.2577 -0.0212 0.083 Uiso 1 1 calc R . .
H10B H 0.8662 -0.1477 0.0146 0.083 Uiso 1 1 calc R . .
C11 C 0.8163(6) -0.3259(6) 0.0057(2) 0.0596(12) Uani 1 1 d . . .
H11A H 0.7821 -0.2938 -0.0421 0.072 Uiso 1 1 calc R . .
H11B H 0.8745 -0.4285 0.0114 0.072 Uiso 1 1 calc R . .
N10 N 0.6740(4) -0.3006(4) 0.05450(16) 0.0427(7) Uani 1 1 d . . .
C12 C 0.5709(6) -0.3804(5) 0.0423(2) 0.0569(11) Uani 1 1 d . . .
H12A H 0.6361 -0.4776 0.0364 0.068 Uiso 1 1 calc R . .
H12B H 0.5136 -0.3331 -0.0001 0.068 Uiso 1 1 calc R . .
C13 C 0.4548(5) -0.3845(5) 0.1039(2) 0.0543(11) Uani 1 1 d . . .
H13A H 0.3829 -0.2879 0.1072 0.065 Uiso 1 1 calc R . .
H13B H 0.3912 -0.4427 0.0987 0.065 Uiso 1 1 calc R . .
N11 N 0.5457(4) -0.4465(3) 0.16745(17) 0.0409(7) Uani 1 1 d . . .
C14 C 0.4418(5) -0.4394(5) 0.2327(2) 0.0517(10) Uani 1 1 d . . .
H14A H 0.3689 -0.4920 0.2325 0.062 Uiso 1 1 calc R . .
H14B H 0.3781 -0.3398 0.2346 0.062 Uiso 1 1 calc R . .
C15 C 0.5387(6) -0.5016(5) 0.2962(2) 0.0567(12) Uani 1 1 d . . .
H15A H 0.6147 -0.5950 0.2899 0.068 Uiso 1 1 calc R . .
H15B H 0.4676 -0.5168 0.3365 0.068 Uiso 1 1 calc R . .
C16 C 0.6295(6) -0.4113(5) 0.3122(2) 0.0532(11) Uani 1 1 d . . .
H16A H 0.5569 -0.3138 0.3125 0.064 Uiso 1 1 calc R . .
H16B H 0.6712 -0.4496 0.3585 0.064 Uiso 1 1 calc R . .
N12 N 0.7642(4) -0.4083(3) 0.25972(15) 0.0400(7) Uani 1 1 d . . .
C17 C 0.8504(6) -0.3146(5) 0.2715(2) 0.0537(11) Uani 1 1 d . . .
H17A H 0.9008 -0.3505 0.3161 0.064 Uiso 1 1 calc R . .
H17B H 0.7767 -0.2176 0.2721 0.064 Uiso 1 1 calc R . .
C18 C 0.9747(5) -0.3149(5) 0.2124(2) 0.0558(11) Uani 1 1 d . . .
H18A H 1.0313 -0.2504 0.2167 0.067 Uiso 1 1 calc R . .
H18B H 1.0520 -0.4110 0.2137 0.067 Uiso 1 1 calc R . .
Cu2 Cu 0.5000 0.0000 0.5000 0.03227(14) Uani 1 2 d S . .
C19 C 0.8282(4) -0.1439(4) 0.4689(2) 0.0453(9) Uani 1 1 d . . .
H19A H 0.8636 -0.1735 0.5166 0.054 Uiso 1 1 calc R . .
H19B H 0.9217 -0.1517 0.4368 0.054 Uiso 1 1 calc R . .
N13 N 0.7166(3) 0.0065(3) 0.45905(15) 0.0343(6) Uani 1 1 d . . .
C20 C 0.7818(5) 0.1049(4) 0.4826(2) 0.0447(9) Uani 1 1 d . . .
H20A H 0.8831 0.1012 0.4569 0.054 Uiso 1 1 calc R . .
H20B H 0.8023 0.0732 0.5321 0.054 Uiso 1 1 calc R . .
C21 C 0.6674(5) 0.2594(5) 0.4713(2) 0.0512(10) Uani 1 1 d . . .
H21A H 0.7228 0.3218 0.4799 0.061 Uiso 1 1 calc R . .
H21B H 0.6396 0.2871 0.4226 0.061 Uiso 1 1 calc R . .
C22 C 0.5150(5) 0.2840(4) 0.5175(2) 0.0479(10) Uani 1 1 d . . .
H22A H 0.5422 0.2457 0.5660 0.057 Uiso 1 1 calc R . .
H22B H 0.4594 0.3867 0.5137 0.057 Uiso 1 1 calc R . .
N14 N 0.4062(4) 0.2157(3) 0.49855(16) 0.0360(7) Uani 1 1 d . . .
C23 C 0.2598(5) 0.2380(4) 0.5453(2) 0.0442(9) Uani 1 1 d . . .
H23A H 0.1923 0.3382 0.5364 0.053 Uiso 1 1 calc R . .
H23B H 0.2878 0.2131 0.5940 0.053 Uiso 1 1 calc R . .
O1 O 0.1915(5) 0.5069(4) 0.4203(2) 0.0933(14) Uani 1 1 d . . .
O2 O 0.7229(8) 0.1194(13) 0.0965(5) 0.246(5) Uani 1 1 d . . .
O3 O 0.4108(13) 0.9731(12) 0.0065(6) 0.119(3) Uiso 0.50 1 d P . .
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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
C6 Mo1 C8 104.04(17) . . ?
C6 Mo1 C7 144.52(17) . . ?
C8 Mo1 C7 83.73(19) . . ?
C6 Mo1 C1 144.15(15) . . ?
C8 Mo1 C1 81.10(16) . . ?
C7 Mo1 C1 70.77(15) . . ?
C6 Mo1 C2 83.04(15) . . ?
C8 Mo1 C2 144.78(16) . . ?
C7 Mo1 C2 110.62(17) . . ?
C1 Mo1 C2 74.30(14) . . ?
C6 Mo1 C4 80.0(2) . . ?
C8 Mo1 C4 144.16(17) . . ?
C7 Mo1 C4 74.6(2) . . ?
C1 Mo1 C4 116.67(16) . . ?
C2 Mo1 C4 70.75(15) . . ?
C6 Mo1 C5 71.77(16) . . ?
C8 Mo1 C5 73.45(15) . . ?
C7 Mo1 C5 142.15(17) . . ?
C1 Mo1 C5 76.07(14) . . ?
C2 Mo1 C5 76.39(14) . . ?
C4 Mo1 C5 138.71(17) . . ?
C6 Mo1 C3 73.78(15) . . ?
C8 Mo1 C3 73.28(17) . . ?
C7 Mo1 C3 75.65(14) . . ?
C1 Mo1 C3 139.52(14) . . ?
C2 Mo1 C3 140.41(15) . . ?
C4 Mo1 C3 73.87(16) . . ?
C5 Mo1 C3 123.51(14) . . ?
N1 C1 Mo1 175.7(3) . . ?
N2 C2 Mo1 178.7(4) . . ?
N3 C3 Mo1 178.3(3) . . ?
N4 C4 Mo1 178.8(5) . . ?
N5 C5 Mo1 178.0(4) . . ?
N6 C6 Mo1 179.0(4) . . ?
N7 C7 Mo1 178.4(5) . . ?
N8 C8 Mo1 176.7(4) . . ?
N12 Cu1 N10 177.23(13) . . ?
N12 Cu1 N9 85.63(14) . . ?
N10 Cu1 N9 93.47(14) . . ?
N12 Cu1 N11 94.82(14) . . ?
N10 Cu1 N11 85.91(14) . . ?
N9 Cu1 N11 176.12(13) . . ?
C18 N9 C9 111.5(3) . . ?
C18 N9 Cu1 107.1(3) . . ?
C9 N9 Cu1 115.2(3) . . ?
N9 C9 C10 111.7(4) . . ?
C9 C10 C11 115.3(4) . . ?
N10 C11 C10 112.8(4) . . ?
C11 N10 C12 110.8(3) . . ?
C11 N10 Cu1 116.6(3) . . ?
C12 N10 Cu1 107.0(3) . . ?
N10 C12 C13 108.6(3) . . ?
N11 C13 C12 108.3(3) . . ?
C13 N11 C14 112.8(3) . . ?
C13 N11 Cu1 105.6(3) . . ?
C14 N11 Cu1 116.6(3) . . ?
N11 C14 C15 111.2(3) . . ?
C14 C15 C16 115.0(4) . . ?
N12 C16 C15 111.7(3) . . ?
C17 N12 C16 113.2(3) . . ?
C17 N12 Cu1 105.5(3) . . ?
C16 N12 Cu1 117.6(3) . . ?
N12 C17 C18 107.2(3) . . ?
N9 C18 C17 108.1(3) . . ?
N13 Cu2 N13 180.00(7) . 2_656 ?
N13 Cu2 N14 85.91(12) . 2_656 ?
N13 Cu2 N14 94.09(12) 2_656 2_656 ?
N13 Cu2 N14 94.09(12) . . ?
N13 Cu2 N14 85.91(12) 2_656 . ?
N14 Cu2 N14 180.00(17) 2_656 . ?
N13 C19 C23 107.8(3) . 2_656 ?
C20 N13 C19 112.3(3) . . ?
C20 N13 Cu2 117.9(2) . . ?
C19 N13 Cu2 107.0(2) . . ?
N13 C20 C21 112.0(3) . . ?
C22 C21 C20 114.4(3) . . ?
N14 C22 C21 112.9(3) . . ?
C23 N14 C22 112.0(3) . . ?
C23 N14 Cu2 105.8(2) . . ?
C22 N14 Cu2 115.9(2) . . ?
N14 C23 C19 108.3(3) . 2_656 ?
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
Mo1 C6 2.139(4) . ?
Mo1 C8 2.145(5) . ?
Mo1 C7 2.150(4) . ?
Mo1 C1 2.154(4) . ?
Mo1 C2 2.157(4) . ?
Mo1 C4 2.159(5) . ?
Mo1 C5 2.170(4) . ?
Mo1 C3 2.171(4) . ?
C1 N1 1.134(5) . ?
C2 N2 1.140(5) . ?
C3 N3 1.145(5) . ?
C4 N4 1.139(6) . ?
C5 N5 1.143(5) . ?
C6 N6 1.134(5) . ?
C7 N7 1.148(6) . ?
C8 N8 1.143(6) . ?
Cu1 N12 2.010(3) . ?
Cu1 N10 2.014(3) . ?
Cu1 N9 2.015(3) . ?
Cu1 N11 2.017(3) . ?
N9 C18 1.471(5) . ?
N9 C9 1.491(5) . ?
C9 C10 1.492(7) . ?
C10 C11 1.507(7) . ?
C11 N10 1.470(5) . ?
N10 C12 1.477(6) . ?
C12 C13 1.491(7) . ?
C13 N11 1.466(5) . ?
N11 C14 1.478(5) . ?
C14 C15 1.494(7) . ?
C15 C16 1.503(7) . ?
C16 N12 1.484(5) . ?
N12 C17 1.470(6) . ?
C17 C18 1.497(7) . ?
Cu2 N13 2.015(3) . ?
Cu2 N13 2.015(3) 2_656 ?
Cu2 N14 2.031(3) 2_656 ?
Cu2 N14 2.031(3) . ?
C19 N13 1.482(5) . ?
C19 C23 1.502(6) 2_656 ?
N13 C20 1.473(5) . ?
C20 C21 1.522(6) . ?
C21 C22 1.508(6) . ?
C22 N14 1.482(5) . ?
N14 C23 1.474(5) . ?
C23 C19 1.502(6) 2_656 ?
