#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/87/2018723.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018723
loop_
_publ_author_name
'Liu, Hou-Ting'
'Lu, Jing'
_publ_section_title
;
 Poly[bis{μ₂-4-[3,5-bis(pyridin-4-yl)phenyl]pyridine}nona-μ₂-oxido-tetraoxidocopper(II)tetramolybdenum(VI)]
;
_journal_coeditor_code           SF3184
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m329
_journal_page_last               m332
_journal_paper_doi               10.1107/S0108270112043648
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu Mo4 O13 (C21 H15 N3)2]'
_chemical_formula_moiety         'C42 H30 Cu Mo4 N6 O13'
_chemical_formula_sum            'C42 H30 Cu Mo4 N6 O13'
_chemical_formula_weight         1274.02
_chemical_name_systematic
;
Poly[bis{μ₂-4-[3,5-bis(pyridin-4-yl)phenyl]pyridine}nona-μ₂-oxido-
tetraoxidocopper(II)tetramolybdenum(VI)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                78.3690(10)
_cell_angle_beta                 83.065(2)
_cell_angle_gamma                76.5010(10)
_cell_formula_units_Z            1
_cell_length_a                   8.1756(4)
_cell_length_b                   9.3263(4)
_cell_length_c                   13.8965(8)
_cell_measurement_reflns_used    3268
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5879
_cell_measurement_theta_min      2.5646
_cell_volume                     1006.13(9)
_computing_cell_refinement       'SMART (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART'
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6181
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.811
_exptl_absorpt_correction_T_max  0.8396
_exptl_absorpt_correction_T_min  0.4962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             625
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.561
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0209P)²+1.7942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0664
_reflns_number_gt                3099
_reflns_number_total             3545
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            sf3184.cif
_cod_data_source_block           I
_cod_database_code               2018723
_cod_database_fobs_code          2018723
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Mo Mo2 0.20305(4) 0.38472(4) -0.04893(2) 0.01664(10) Uani d . 1 1
Mo Mo1 0.33602(4) 0.67904(4) 0.07478(2) 0.01823(10) Uani d . 1 1
Cu Cu1 0.0000 1.0000 0.0000 0.02298(17) Uani d S 1 2
O O1 0.1353(3) 0.2255(3) -0.0509(2) 0.0282(6) Uani d . 1 1
O O2 0.0000 0.5000 0.0000 0.0304(10) Uani d S 1 2
O O3 0.2044(4) 0.4709(3) -0.1681(2) 0.0356(7) Uani d . 1 1
O O4 0.3040(3) 0.5490(3) 0.0063(2) 0.0257(6) Uani d . 1 1
O O5 0.5501(3) 0.7066(3) 0.0583(2) 0.0275(6) Uani d . 1 1
O O6 0.2857(4) 0.6190(4) 0.1958(2) 0.0413(8) Uani d . 1 1
O O7 0.2045(3) 0.8534(3) 0.0382(2) 0.0256(6) Uani d . 1 1
N N1 0.2561(4) 0.2517(4) 0.1187(2) 0.0230(7) Uani d . 1 1
N N2 0.9111(5) -0.6487(4) 0.4850(3) 0.0406(10) Uani d . 1 1
N N3 0.0659(4) -0.0251(4) 0.8585(2) 0.0230(7) Uani d . 1 1
C C1 0.3405(6) 0.1089(5) 0.1263(3) 0.0370(11) Uani d . 1 1
H H1 0.3808 0.0722 0.0686 0.044 Uiso calc R 1 1
C C2 0.3708(6) 0.0139(5) 0.2143(3) 0.0397(12) Uani d . 1 1
H H2 0.4297 -0.0845 0.2151 0.048 Uiso calc R 1 1
C C3 0.3135(5) 0.0647(4) 0.3022(3) 0.0228(8) Uani d . 1 1
C C4 0.2259(5) 0.2123(5) 0.2942(3) 0.0272(9) Uani d . 1 1
H H4 0.1840 0.2521 0.3507 0.033 Uiso calc R 1 1
C C5 0.2007(5) 0.3005(5) 0.2027(3) 0.0257(9) Uani d . 1 1
H H5 0.1419 0.3993 0.1996 0.031 Uiso calc R 1 1
C C6 0.3465(5) -0.0361(4) 0.3987(3) 0.0217(8) Uani d . 1 1
C C7 0.4711(4) -0.1617(4) 0.3996(3) 0.0149(7) Uani d . 1 1
H H7 0.5305 -0.1834 0.3411 0.018 Uiso calc R 1 1
C C8 0.5085(5) -0.2554(4) 0.4863(3) 0.0213(8) Uani d . 1 1
C C9 0.4240(4) -0.2248(4) 0.5728(2) 0.0152(7) Uani d . 1 1
H H9 0.4523 -0.2892 0.6316 0.018 Uiso calc R 1 1
C C10 0.2978(5) -0.0998(4) 0.5736(3) 0.0221(8) Uani d . 1 1
C C11 0.2569(5) -0.0043(4) 0.4860(3) 0.0219(8) Uani d . 1 1
H H11 0.1701 0.0804 0.4855 0.026 Uiso calc R 1 1
C C12 0.8237(5) -0.6137(5) 0.5673(4) 0.0377(11) Uani d . 1 1
H H12 0.8520 -0.6778 0.6263 0.045 Uiso calc R 1 1
C C13 0.6940(5) -0.4892(5) 0.5719(3) 0.0303(10) Uani d . 1 1
H H13 0.6392 -0.4711 0.6323 0.036 Uiso calc R 1 1
C C14 0.6467(5) -0.3923(4) 0.4860(3) 0.0213(8) Uani d . 1 1
C C15 0.7340(5) -0.4288(5) 0.3990(3) 0.0305(10) Uani d . 1 1
H H15 0.7060 -0.3688 0.3386 0.037 Uiso calc R 1 1
C C16 0.8623(5) -0.5547(5) 0.4032(4) 0.0383(11) Uani d . 1 1
H H16 0.9196 -0.5757 0.3439 0.046 Uiso calc R 1 1
C C17 0.0649(5) 0.0889(5) 0.7828(3) 0.0294(10) Uani d . 1 1
H H17 0.0155 0.1853 0.7936 0.035 Uiso calc R 1 1
C C18 0.1339(5) 0.0702(5) 0.6892(3) 0.0266(9) Uani d . 1 1
H H18 0.1291 0.1529 0.6386 0.032 Uiso calc R 1 1
C C19 0.2104(5) -0.0720(4) 0.6707(3) 0.0222(8) Uani d . 1 1
C C20 0.2047(6) -0.1905(5) 0.7489(3) 0.0302(10) Uani d . 1 1
H H20 0.2509 -0.2884 0.7398 0.036 Uiso calc R 1 1
C C21 0.1308(5) -0.1634(5) 0.8397(3) 0.0280(9) Uani d . 1 1
H H21 0.1257 -0.2447 0.8903 0.034 Uiso calc R 1 1
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'
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'
N N 0.0061 0.0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Mo2 O1 . . 103.23(14) y
O3 Mo2 O2 . . 99.11(10) y
O1 Mo2 O2 . . 99.07(9) y
O3 Mo2 O5 . 2_665 93.60(13) y
O1 Mo2 O5 . 2_665 96.61(12) y
O2 Mo2 O5 . 2_665 156.94(8) y
O3 Mo2 O4 . . 96.56(13) y
O1 Mo2 O4 . . 160.02(12) y
O2 Mo2 O4 . . 80.25(7) y
O5 Mo2 O4 2_665 . 79.24(10) y
O3 Mo2 N1 . . 169.75(13) y
O1 Mo2 N1 . . 80.32(12) y
O2 Mo2 N1 . . 89.72(7) y
O5 Mo2 N1 2_665 . 76.36(11) y
O4 Mo2 N1 . . 79.71(10) y
O6 Mo1 O7 . . 108.18(14) y
O6 Mo1 O4 . . 108.97(14) y
O7 Mo1 O4 . . 109.97(12) y
O6 Mo1 O5 . . 109.50(14) y
O7 Mo1 O5 . . 107.06(13) y
O4 Mo1 O5 . . 113.05(12) y
O7 Cu1 O7 . 2_575 180.0000(10) ?
O7 Cu1 N3 . 2_566 90.98(12) y
O7 Cu1 N3 2_575 2_566 89.02(12) y
O7 Cu1 N3 . 1_564 89.02(12) y
O7 Cu1 N3 2_575 1_564 90.98(12) y
N3 Cu1 N3 2_566 1_564 180.0000(10) ?
O1 Cu1 N3 2_565 2_566 83.40(12) y
O1 Cu1 O7 2_565 . 83.20(11) y
O1 Cu1 N3 2_565 1_564 96.60(11) y
O1 Cu1 O7 2_565 2_575 96.80(10) y
Mo2 O2 Mo2 2_565 . 180.000(18) ?
Mo1 O4 Mo2 . . 164.00(15) ?
Mo1 O5 Mo2 . 2_665 147.98(16) ?
Mo1 O7 Cu1 . . 158.80(16) ?
C5 N1 C1 . . 116.4(3) ?
C5 N1 Mo2 . . 127.8(3) ?
C1 N1 Mo2 . . 115.6(3) ?
C16 N2 C12 . . 114.6(4) ?
C17 N3 C21 . . 117.2(3) ?
C17 N3 Cu1 . 1_546 124.0(3) ?
C21 N3 Cu1 . 1_546 118.5(3) ?
N1 C1 C2 . . 123.8(4) ?
N1 C1 H1 . . 118.1 ?
C2 C1 H1 . . 118.1 ?
C1 C2 C3 . . 119.9(4) ?
C1 C2 H2 . . 120.0 ?
C3 C2 H2 . . 120.0 ?
C4 C3 C2 . . 116.3(4) ?
C4 C3 C6 . . 122.8(3) ?
C2 C3 C6 . . 120.9(4) ?
C5 C4 C3 . . 120.1(4) ?
C5 C4 H4 . . 119.9 ?
C3 C4 H4 . . 119.9 ?
N1 C5 C4 . . 123.5(4) ?
N1 C5 H5 . . 118.3 ?
C4 C5 H5 . . 118.3 ?
C7 C6 C11 . . 120.1(3) ?
C7 C6 C3 . . 117.7(3) ?
C11 C6 C3 . . 122.3(3) ?
C8 C7 C6 . . 119.9(3) ?
C8 C7 H7 . . 120.1 ?
C6 C7 H7 . . 120.1 ?
C7 C8 C9 . . 120.9(3) ?
C7 C8 C14 . . 119.1(3) ?
C9 C8 C14 . . 120.0(3) ?
C8 C9 C10 . . 120.2(3) ?
C8 C9 H9 . . 119.9 ?
C10 C9 H9 . . 119.9 ?
C9 C10 C11 . . 119.6(3) ?
C9 C10 C19 . . 117.7(3) ?
C11 C10 C19 . . 122.7(3) ?
C10 C11 C6 . . 119.4(4) ?
C10 C11 H11 . . 120.3 ?
C6 C11 H11 . . 120.3 ?
N2 C12 C13 . . 125.0(4) ?
N2 C12 H12 . . 117.5 ?
C13 C12 H12 . . 117.5 ?
C14 C13 C12 . . 119.3(4) ?
C14 C13 H13 . . 120.3 ?
C12 C13 H13 . . 120.3 ?
C13 C14 C15 . . 116.5(4) ?
C13 C14 C8 . . 121.8(4) ?
C15 C14 C8 . . 121.6(4) ?
C16 C15 C14 . . 119.2(4) ?
C16 C15 H15 . . 120.4 ?
C14 C15 H15 . . 120.4 ?
N2 C16 C15 . . 125.4(4) ?
N2 C16 H16 . . 117.3 ?
C15 C16 H16 . . 117.3 ?
N3 C17 C18 . . 123.0(4) ?
N3 C17 H17 . . 118.5 ?
C18 C17 H17 . . 118.5 ?
C17 C18 C19 . . 120.0(4) ?
C17 C18 H18 . . 120.0 ?
C19 C18 H18 . . 120.0 ?
C18 C19 C20 . . 116.5(4) ?
C18 C19 C10 . . 123.1(4) ?
C20 C19 C10 . . 120.4(3) ?
C21 C20 C19 . . 120.1(4) ?
C21 C20 H20 . . 119.9 ?
C19 C20 H20 . . 119.9 ?
N3 C21 C20 . . 123.0(4) ?
N3 C21 H21 . . 118.5 ?
C20 C21 H21 . . 118.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo2 O3 . 1.689(3) y
Mo2 O1 . 1.708(3) y
Mo2 O2 . 1.8876(3) y
Mo2 O5 2_665 1.999(2) y
Mo2 O4 . 2.199(3) y
Mo2 N1 . 2.445(3) y
Mo1 O6 . 1.695(3) y
Mo1 O7 . 1.744(3) y
Mo1 O4 . 1.766(3) y
Mo1 O5 . 1.808(3) y
Cu1 O7 . 1.950(3) y
Cu1 O7 2_575 1.950(3) ?
Cu1 N3 2_566 2.021(3) y
Cu1 N3 1_564 2.021(3) ?
Cu1 O1 2_565 2.538(3) y
O2 Mo2 2_565 1.8876(3) ?
O5 Mo2 2_665 1.999(2) ?
N1 C5 . 1.329(5) ?
N1 C1 . 1.338(5) ?
N2 C16 . 1.328(6) ?
N2 C12 . 1.331(6) ?
N3 C17 . 1.336(5) ?
N3 C21 . 1.340(5) ?
N3 Cu1 1_546 2.021(3) ?
C1 C2 . 1.369(6) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.388(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.385(5) ?
C3 C6 . 1.489(5) ?
C4 C5 . 1.377(5) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C6 C7 . 1.360(5) ?
C6 C11 . 1.387(5) ?
C7 C8 . 1.360(5) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.360(5) ?
C8 C14 . 1.494(5) ?
C9 C10 . 1.366(5) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.381(5) ?
C10 C19 . 1.490(5) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.384(6) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.381(5) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.389(5) ?
C15 C16 . 1.377(6) ?
C15 H15 . 0.9300 ?
C16 H16 . 0.9300 ?
C17 C18 . 1.382(5) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.389(5) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.390(5) ?
C20 C21 . 1.377(5) ?
C20 H20 . 0.9300 ?
C21 H21 . 0.9300 ?
