#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/15/2231572.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_2231572
loop_
_publ_author_name
'Han, Li-Juan'
_publ_section_title
;
 catena-Poly[[tetrakis(μ-pentafluorobenzoato-κ²O:O')dimolybdenum(II)]-μ-4,4'-bipyridine-κ²N:N']
;
_journal_coeditor_code           JJ2094
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1235
_journal_page_last               m1236
_journal_paper_doi               10.1107/S1600536811031734
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mo2 (C7 F5 O2)4 (C10 H8 N2)]'
_chemical_formula_moiety         'C28 F20 Mo2 O8, C10 H8 N2'
_chemical_formula_sum            'C38 H8 F20 Mo2 N2 O8'
_chemical_formula_weight         1192.34
_chemical_name_common            Mo2(OOCC6F5)4(C10H8N2)
_chemical_name_systematic
;
catena-Poly[[tetrakis(μ-pentafluorobenzoato-
κ²O:O')dimolybdenum(II)]-μ-4,4'-bipyridine-
κ²N:N']
;
_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                101.1580(10)
_cell_angle_beta                 94.6970(10)
_cell_angle_gamma                99.0920(10)
_cell_formula_units_Z            1
_cell_length_a                   8.8858(8)
_cell_length_b                   9.9311(9)
_cell_length_c                   11.1978(10)
_cell_measurement_reflns_used    4122
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.52
_cell_volume                     950.83(15)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEXII CCD '
_diffrn_measurement_method       ω
_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  0.0128
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4937
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.465
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0239
_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)+(0.0323P)²+0.6373P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                3072
_reflns_number_total             3294
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jj2094.cif
_cod_data_source_block           I
_cod_database_code               2231572
_cod_database_fobs_code          2231572
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 Mo1 0.94356(2) 0.58128(2) 0.480838(17) 0.02757(8) Uani d . 1 1
F F11 0.46291(19) 0.34697(17) 0.29542(17) 0.0569(4) Uani d . 1 1
F F12 0.2509(2) 0.1493(2) 0.1523(2) 0.0712(5) Uani d . 1 1
F F13 0.3174(2) -0.10294(19) 0.05942(18) 0.0682(5) Uani d . 1 1
F F14 0.6015(2) -0.15799(17) 0.11139(18) 0.0662(5) Uani d . 1 1
F F15 0.81465(19) 0.03236(17) 0.25713(17) 0.0568(4) Uani d . 1 1
F F31 1.0522(2) 0.7439(2) 0.89717(17) 0.0701(5) Uani d . 1 1
F F32 0.9848(3) 0.8073(2) 1.13037(18) 0.0825(6) Uani d . 1 1
F F33 0.7539(2) 0.6435(2) 1.20533(14) 0.0708(6) Uani d . 1 1
F F34 0.5986(3) 0.4110(2) 1.05142(19) 0.0823(6) Uani d . 1 1
F F35 0.6643(2) 0.3488(2) 0.81764(17) 0.0770(6) Uani d . 1 1
O O1 0.75702(18) 0.43333(16) 0.38004(15) 0.0332(4) Uani d . 1 1
O O2 0.87528(19) 0.26377(17) 0.42436(15) 0.0345(4) Uani d . 1 1
O O5 0.85431(19) 0.59500(18) 0.65400(15) 0.0355(4) Uani d . 1 1
O O6 1.03083(19) 0.58024(17) 0.31053(15) 0.0352(4) Uani d . 1 1
C C1 0.7665(3) 0.3051(3) 0.3681(2) 0.0330(5) Uani d . 1 1
C C3 0.8955(3) 0.5167(3) 0.7219(2) 0.0325(5) Uani d . 1 1
C C11 0.6483(3) 0.1984(3) 0.2857(2) 0.0341(5) Uani d . 1 1
C C12 0.5018(3) 0.2234(3) 0.2528(2) 0.0391(6) Uani d . 1 1
C C13 0.3913(3) 0.1235(3) 0.1796(3) 0.0456(7) Uani d . 1 1
C C14 0.4231(3) -0.0065(3) 0.1325(3) 0.0467(7) Uani d . 1 1
C C15 0.5677(3) -0.0340(3) 0.1609(2) 0.0437(6) Uani d . 1 1
C C16 0.6762(3) 0.0656(3) 0.2357(2) 0.0382(6) Uani d . 1 1
C C31 0.8594(3) 0.5460(3) 0.8527(2) 0.0346(5) Uani d . 1 1
C C32 0.9392(3) 0.6610(3) 0.9340(2) 0.0428(6) Uani d . 1 1
C C33 0.9070(4) 0.6945(3) 1.0538(2) 0.0497(7) Uani d . 1 1
C C34 0.7909(3) 0.6100(3) 1.0917(2) 0.0480(7) Uani d . 1 1
C C35 0.7115(3) 0.4929(3) 1.0133(3) 0.0502(7) Uani d . 1 1
C C36 0.7458(3) 0.4611(3) 0.8941(2) 0.0437(6) Uani d . 1 1
N N1 0.2434(3) 0.2426(2) 0.5169(2) 0.0434(5) Uani d . 1 1
C C51 0.3883(4) 0.2800(3) 0.5640(2) 0.0498(7) Uani d . 1 1
H H51A 0.4226 0.3727 0.6027 0.060 Uiso calc R 1 1
C C52 0.1981(3) 0.1097(3) 0.4617(3) 0.0555(8) Uani d . 1 1
H H52A 0.0966 0.0810 0.4270 0.067 Uiso calc R 1 1
C C53 0.2934(3) 0.0113(3) 0.4527(3) 0.0540(8) Uani d . 1 1
H H53A 0.2554 -0.0805 0.4130 0.065 Uiso calc R 1 1
C C54 0.4463(3) 0.0507(3) 0.5034(2) 0.0377(6) Uani d . 1 1
C C55 0.4927(3) 0.1900(3) 0.5594(2) 0.0467(7) Uani d . 1 1
H H55A 0.5938 0.2230 0.5938 0.056 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'
F F 0.0171 0.0103 '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'
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'
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
O2 Mo1 O1 2_766 . 176.82(6)
O2 Mo1 O6 2_766 . 92.90(7)
O1 Mo1 O6 . . 85.79(7)
O2 Mo1 Mo1 2_766 2_766 92.41(4)
O1 Mo1 Mo1 . 2_766 90.57(4)
O6 Mo1 Mo1 . 2_766 93.70(4)
O2 Mo1 O5 2_766 . 85.43(7)
O1 Mo1 O5 . . 95.73(7)
O6 Mo1 O5 . . 176.63(6)
Mo1 Mo1 O5 2_766 . 89.29(4)
C1 O1 Mo1 . . 117.52(15)
C1 O2 Mo1 . 2_766 116.51(15)
C3 O5 Mo1 . . 117.24(14)
C3 O6 Mo1 2_766 . 114.32(14)
O1 C1 O2 . . 122.5(2)
O1 C1 C11 . . 119.5(2)
O2 C1 C11 . . 118.0(2)
O5 C3 O6 . 2_766 124.7(2)
O5 C3 C31 . . 117.2(2)
O6 C3 C31 2_766 . 118.1(2)
C12 C11 C16 . . 115.6(2)
C12 C11 C1 . . 122.4(2)
C16 C11 C1 . . 122.0(2)
F11 C12 C13 . . 117.1(2)
F11 C12 C11 . . 120.6(2)
C13 C12 C11 . . 122.3(2)
F12 C13 C12 . . 121.0(3)
F12 C13 C14 . . 118.7(3)
C12 C13 C14 . . 120.3(2)
F13 C14 C15 . . 120.5(3)
F13 C14 C13 . . 120.6(3)
C15 C14 C13 . . 119.0(3)
F14 C15 C16 . . 120.4(2)
F14 C15 C14 . . 119.3(3)
C16 C15 C14 . . 120.3(2)
F15 C16 C15 . . 116.8(2)
F15 C16 C11 . . 120.6(2)
C15 C16 C11 . . 122.5(2)
C32 C31 C36 . . 118.0(2)
C32 C31 C3 . . 119.8(2)
C36 C31 C3 . . 122.2(2)
F31 C32 C31 . . 119.4(2)
F31 C32 C33 . . 118.7(3)
C31 C32 C33 . . 121.9(3)
F32 C33 C34 . . 120.4(3)
F32 C33 C32 . . 120.8(3)
C34 C33 C32 . . 118.9(3)
F33 C34 C35 . . 119.8(3)
F33 C34 C33 . . 119.8(3)
C35 C34 C33 . . 120.5(2)
F34 C35 C34 . . 119.9(3)
F34 C35 C36 . . 120.3(3)
C34 C35 C36 . . 119.8(3)
F35 C36 C31 . . 119.9(2)
F35 C36 C35 . . 119.0(3)
C31 C36 C35 . . 121.0(3)
C51 N1 C52 . . 116.5(2)
N1 C51 C55 . . 124.1(3)
N1 C51 H51A . . 117.9
C55 C51 H51A . . 117.9
N1 C52 C53 . . 123.8(3)
N1 C52 H52A . . 118.1
C53 C52 H52A . . 118.1
C52 C53 C54 . . 119.7(3)
C52 C53 H53A . . 120.2
C54 C53 H53A . . 120.2
C55 C54 C53 . . 116.0(2)
C55 C54 C54 . 2_656 122.0(3)
C53 C54 C54 . 2_656 122.0(3)
C51 C55 C54 . . 119.9(3)
C51 C55 H55A . . 120.1
C54 C55 H55A . . 120.1
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
Mo1 O2 2_766 2.0955(17) ?
Mo1 O1 . 2.1124(17) y
Mo1 O6 . 2.1155(16) y
Mo1 Mo1 2_766 2.1227(4) y
Mo1 O5 . 2.1427(16) y
Mo1 N1 2_666 2.594(2) ?
F11 C12 . 1.337(3) ?
F12 C13 . 1.335(3) ?
F13 C14 . 1.325(3) ?
F14 C15 . 1.340(3) ?
F15 C16 . 1.338(3) ?
F31 C32 . 1.338(3) ?
F32 C33 . 1.325(3) ?
F33 C34 . 1.333(3) ?
F34 C35 . 1.341(3) ?
F35 C36 . 1.333(3) ?
O1 C1 . 1.272(3) ?
O2 C1 . 1.274(3) ?
O2 Mo1 2_766 2.0955(17) ?
O5 C3 . 1.261(3) ?
O6 C3 2_766 1.261(3) ?
C1 C11 . 1.480(3) ?
C3 O6 2_766 1.261(3) ?
C3 C31 . 1.508(3) ?
C11 C12 . 1.397(3) ?
C11 C16 . 1.398(3) ?
C12 C13 . 1.366(4) ?
C13 C14 . 1.379(4) ?
C14 C15 . 1.379(4) ?
C15 C16 . 1.362(4) ?
C31 C32 . 1.368(4) ?
C31 C36 . 1.379(4) ?
C32 C33 . 1.383(4) ?
C33 C34 . 1.373(4) ?
C34 C35 . 1.365(4) ?
C35 C36 . 1.381(4) ?
N1 C51 . 1.318(4) ?
N1 C52 . 1.327(4) ?
C51 C55 . 1.383(4) ?
C51 H51A . 0.9300 ?
C52 C53 . 1.385(4) ?
C52 H52A . 0.9300 ?
C53 C54 . 1.393(4) ?
C53 H53A . 0.9300 ?
C54 C55 . 1.385(4) ?
C54 C54 2_656 1.489(5) ?
C55 H55A . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C55 H55A F35 1_555 0.93 2.55 3.152(2) 122.40 y
C51 H51A F33 2_667 0.93 2.78 2.987(3) 93.86 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O6 Mo1 O1 C1 . . 91.22(16) ?
Mo1 Mo1 O1 C1 2_766 . -2.45(16) ?
O5 Mo1 O1 C1 . . -91.80(16) ?
O2 Mo1 O5 C3 2_766 . -89.66(18) ?
O1 Mo1 O5 C3 . . 93.32(18) ?
Mo1 Mo1 O5 C3 2_766 . 2.82(18) ?
O2 Mo1 O6 C3 2_766 2_766 98.99(17) ?
O1 Mo1 O6 C3 . 2_766 -83.91(17) ?
Mo1 Mo1 O6 C3 2_766 2_766 6.38(17) ?
Mo1 O1 C1 O2 . . 7.3(3) ?
Mo1 O1 C1 C11 . . -172.39(15) ?
Mo1 O2 C1 O1 2_766 . -8.4(3) ?
Mo1 O2 C1 C11 2_766 . 171.27(15) ?
Mo1 O5 C3 O6 . 2_766 -9.2(3) ?
Mo1 O5 C3 C31 . . 168.03(16) ?
O1 C1 C11 C12 . . -22.4(3) y
O2 C1 C11 C12 . . 157.9(2) ?
O1 C1 C11 C16 . . 157.6(2) ?
O2 C1 C11 C16 . . -22.1(3) y
C16 C11 C12 F11 . . -179.9(2) ?
C1 C11 C12 F11 . . 0.0(4) ?
C16 C11 C12 C13 . . 2.0(4) ?
C1 C11 C12 C13 . . -178.1(2) ?
F11 C12 C13 F12 . . 0.0(4) ?
C11 C12 C13 F12 . . 178.2(2) ?
F11 C12 C13 C14 . . -179.9(2) ?
C11 C12 C13 C14 . . -1.8(4) ?
F12 C13 C14 F13 . . 1.4(4) ?
C12 C13 C14 F13 . . -178.6(2) ?
F12 C13 C14 C15 . . -179.6(3) ?
C12 C13 C14 C15 . . 0.3(4) ?
F13 C14 C15 F14 . . 1.7(4) ?
C13 C14 C15 F14 . . -177.2(3) ?
F13 C14 C15 C16 . . 179.7(2) ?
C13 C14 C15 C16 . . 0.8(4) ?
F14 C15 C16 F15 . . -0.7(4) ?
C14 C15 C16 F15 . . -178.7(2) ?
F14 C15 C16 C11 . . 177.5(2) ?
C14 C15 C16 C11 . . -0.5(4) ?
C12 C11 C16 F15 . . 177.3(2) ?
C1 C11 C16 F15 . . -2.7(4) ?
C12 C11 C16 C15 . . -0.8(4) ?
C1 C11 C16 C15 . . 179.2(2) ?
O5 C3 C31 C32 . . -72.1(3) y
O6 C3 C31 C32 2_766 . 105.4(3) ?
O5 C3 C31 C36 . . 107.0(3) ?
O6 C3 C31 C36 2_766 . -75.6(3) y
C36 C31 C32 F31 . . 178.7(2) ?
C3 C31 C32 F31 . . -2.2(4) ?
C36 C31 C32 C33 . . -1.2(4) ?
C3 C31 C32 C33 . . 177.9(2) ?
F31 C32 C33 F32 . . 0.9(4) ?
C31 C32 C33 F32 . . -179.3(3) ?
F31 C32 C33 C34 . . 179.8(2) ?
C31 C32 C33 C34 . . -0.3(4) ?
F32 C33 C34 F33 . . 1.7(4) ?
C32 C33 C34 F33 . . -177.3(2) ?
F32 C33 C34 C35 . . -179.4(3) ?
C32 C33 C34 C35 . . 1.7(4) ?
F33 C34 C35 F34 . . -1.1(4) ?
C33 C34 C35 F34 . . 179.9(3) ?
F33 C34 C35 C36 . . 177.4(3) ?
C33 C34 C35 C36 . . -1.5(4) ?
C32 C31 C36 F35 . . 179.4(2) ?
C3 C31 C36 F35 . . 0.3(4) ?
C32 C31 C36 C35 . . 1.3(4) ?
C3 C31 C36 C35 . . -177.8(2) ?
F34 C35 C36 F35 . . 0.5(4) ?
C34 C35 C36 F35 . . -178.0(3) ?
F34 C35 C36 C31 . . 178.6(3) ?
C34 C35 C36 C31 . . 0.0(4) ?
C52 N1 C51 C55 . . -0.3(4) ?
C51 N1 C52 C53 . . 0.6(4) ?
N1 C52 C53 C54 . . -0.1(5) ?
C52 C53 C54 C55 . . -0.7(4) ?
C52 C53 C54 C54 . 2_656 179.9(3) ?
N1 C51 C55 C54 . . -0.5(4) ?
C53 C54 C55 C51 . . 1.0(4) ?
C54 C54 C55 C51 2_656 . -179.6(3) ?
