#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/19/7221906.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_7221906
loop_
_publ_author_name
'Du, Hai-Juan'
'Wang, Chao-Hai'
'Li, Yao'
'Niu, Yunyin'
'Hou, Hongwei'
_publ_section_title
;
 Four hybrid compounds based on new type of molybdates and a flexible
 tripodal ligand: synthesis, structures, photochemical and electrochemical
 properties
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA13007G
_journal_year                    2015
_chemical_formula_moiety
'Mo8 O26, Co H4 Mo8 O28, 4.5(H2 O), 2(C21 H27 N6)'
_chemical_formula_sum            'C42 H67 Co Mo16 N12 O58.5'
_chemical_formula_weight         3270.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-01 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                100.614(4)
_cell_angle_beta                 96.093(4)
_cell_angle_gamma                103.887(4)
_cell_formula_units_Z            1
_cell_length_a                   10.7586(5)
_cell_length_b                   11.3075(4)
_cell_length_c                   17.9670(9)
_cell_measurement_reflns_used    8209
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.9890
_cell_measurement_theta_min      3.2380
_cell_volume                     2059.49(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   28.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323   77.0000  -90.0000 25

  2 omega  -45.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323   77.0000   30.0000 90

  3 omega  -10.00   83.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000  150.0000 93

  4 omega    4.00   66.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000    0.0000 62

  5 omega   64.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000 -180.0000 26

  6 omega   -8.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   77.0000  -90.0000 96

  7 omega   32.00   80.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104 -178.0000  -30.0000 48
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0364760000
_diffrn_orient_matrix_UB_12      0.0563889000
_diffrn_orient_matrix_UB_13      0.0253626000
_diffrn_orient_matrix_UB_21      0.0503258000
_diffrn_orient_matrix_UB_22      -0.0284449000
_diffrn_orient_matrix_UB_23      0.0083249000
_diffrn_orient_matrix_UB_31      0.0294364000
_diffrn_orient_matrix_UB_32      0.0198305000
_diffrn_orient_matrix_UB_33      -0.0306877000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17103
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.030
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.637
_exptl_crystal_F_000             1570
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.599
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8405
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0246P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7032
_reflns_number_total             8405
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ra13007g2.cif
_cod_data_source_block           nyy14060304
_cod_original_cell_volume        2059.51(16)
_cod_original_formula_sum        'C42 H67 Co Mo16 N12 O58.50'
_cod_database_code               7221906
#BEGIN Tags that were not found in dictionaries:
_chemical_oxdiff_formula         C1H1O1N1Cl2Cd1Mo1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.647
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O30(0.25) H30A(0.25) H30B(0.25)
4.a Riding coordinates:
 O30(H30A,H30B), O29(H29A,H29B)
4.b Free rotating group:
 O28(H28A,H28B)
4.c Rotating group:
 O27(H27A,H27B)
4.d Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B)
4.e Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21)
4.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mo1 Mo -0.27684(4) 0.06557(4) -0.05856(2) 0.02128(10) Uani 1 1 d . . .
Mo2 Mo -0.04720(4) 0.27968(3) 0.07440(2) 0.02151(10) Uani 1 1 d . . .
Mo3 Mo 0.23105(4) 0.21411(3) 0.13160(2) 0.02094(10) Uani 1 1 d . . .
Mo4 Mo -0.07382(4) -0.06612(3) 0.07728(2) 0.01668(9) Uani 1 1 d . . .
O1 O -0.3877(3) 0.0995(3) -0.0029(2) 0.0315(8) Uani 1 1 d . . .
O2 O -0.3335(3) 0.0787(3) -0.1473(2) 0.0337(8) Uani 1 1 d . . .
O3 O -0.1421(3) 0.2186(3) -0.02712(17) 0.0233(7) Uani 1 1 d . . .
O4 O 0.0424(3) 0.4228(3) 0.06667(19) 0.0336(8) Uani 1 1 d . . .
O5 O -0.1630(3) 0.3079(3) 0.1275(2) 0.0321(8) Uani 1 1 d . . .
O6 O -0.1449(3) 0.0547(3) 0.05708(18) 0.0238(7) Uani 1 1 d . . .
O7 O 0.0641(3) 0.2364(3) 0.14769(17) 0.0224(7) Uani 1 1 d . . .
O8 O 0.3157(3) 0.3581(3) 0.1239(2) 0.0319(8) Uani 1 1 d . . .
O9 O 0.3136(3) 0.1106(3) 0.06850(18) 0.0236(7) Uani 1 1 d . . .
O10 O 0.2888(3) 0.1987(3) 0.22000(19) 0.0327(8) Uani 1 1 d . . .
O11 O 0.0976(3) -0.0033(3) 0.10709(18) 0.0256(8) Uani 1 1 d . . .
O12 O -0.1419(3) -0.1263(3) 0.14846(19) 0.0302(8) Uani 1 1 d . . .
O13 O -0.1042(3) -0.1868(3) -0.00699(18) 0.0244(7) Uani 1 1 d . . .
Mo5 Mo 0.23640(4) 0.52328(3) 0.36446(2) 0.01721(9) Uani 1 1 d . . .
Mo6 Mo 0.52785(3) 0.45609(3) 0.40416(2) 0.01359(9) Uani 1 1 d . . .
Mo7 Mo 0.53632(4) 0.26159(3) 0.51329(2) 0.01620(9) Uani 1 1 d . . .
Mo8 Mo 0.24654(3) 0.33042(3) 0.47728(2) 0.01571(9) Uani 1 1 d . . .
Co1 Co 0.0000 0.5000 0.5000 0.01905(19) Uani 1 2 d S T P
O14 O 0.1206(3) 0.5593(3) 0.41871(18) 0.0225(7) Uani 1 1 d . . .
O15 O 0.1701(3) 0.5088(3) 0.27265(18) 0.0292(8) Uani 1 1 d . . .
O16 O 0.3624(3) 0.6814(2) 0.38672(17) 0.0196(7) Uani 1 1 d . . .
O17 O 0.4114(3) 0.4669(2) 0.33177(17) 0.0180(7) Uani 1 1 d . . .
O18 O 0.6394(3) 0.4044(3) 0.35709(17) 0.0207(7) Uani 1 1 d . . .
O19 O 0.6151(3) 0.4716(2) 0.51910(16) 0.0161(6) Uani 1 1 d . . .
O20 O 0.4294(3) 0.3007(2) 0.42726(16) 0.0165(6) Uani 1 1 d . . .
O21 O 0.6470(3) 0.2178(3) 0.46017(18) 0.0263(8) Uani 1 1 d . . .
O22 O 0.4362(3) 0.1257(3) 0.52198(18) 0.0261(8) Uani 1 1 d . . .
O23 O 0.3883(3) 0.3649(2) 0.56437(16) 0.0154(6) Uani 1 1 d . . .
O24 O 0.1814(3) 0.1751(3) 0.46574(19) 0.0266(8) Uani 1 1 d . . .
O25 O 0.1394(3) 0.4002(3) 0.52229(18) 0.0209(7) Uani 1 1 d . . .
O26 O 0.2013(3) 0.3530(3) 0.37714(17) 0.0204(7) Uani 1 1 d . . .
O27 O -0.1083(3) 0.3471(3) 0.42198(19) 0.0311(8) Uani 1 1 d . . .
H27A H -0.1524 0.2959 0.4451 0.047 Uiso 1 1 d GR . .
H27B H -0.0581 0.3119 0.3977 0.047 Uiso 1 1 d GR . .
O30 O 0.405(3) 0.200(3) 0.9437(19) 0.173(13) Uani 0.25 1 d . U .
H30A H 0.4311 0.1307 0.9592 0.260 Uiso 0.25 1 d R . .
H30B H 0.3225 0.1716 0.9488 0.260 Uiso 0.25 1 d R . .
O29 O 0.0663(6) 0.6876(4) 0.1625(3) 0.101(2) Uani 1 1 d . . .
H29A H 0.0903 0.6274 0.1614 0.151 Uiso 1 1 d R . .
H29B H 0.0864 0.7063 0.1208 0.151 Uiso 1 1 d R . .
O28 O -0.0553(5) 0.2242(5) 0.2885(3) 0.0775(16) Uani 1 1 d . . .
H28A H 0.0271 0.2437 0.2966 0.116 Uiso 1 1 d G . .
H28B H -0.0818 0.2134 0.2408 0.116 Uiso 1 1 d G . .
N1 N 0.3990(4) -0.0106(3) 0.7391(2) 0.0234(9) Uani 1 1 d . . .
N2 N 0.3713(4) -0.0755(4) 0.8424(3) 0.0366(11) Uani 1 1 d . . .
H2 H 0.3536 -0.0787 0.8877 0.044 Uiso 1 1 calc R . .
N3 N -0.0929(4) 0.1237(3) 0.6421(2) 0.0243(9) Uani 1 1 d . . .
N4 N -0.1969(5) 0.0053(4) 0.7068(3) 0.0502(13) Uani 1 1 d . . .
H4 H -0.2139 -0.0366 0.7416 0.060 Uiso 1 1 calc R . .
N5 N 0.3467(4) 0.5056(3) 0.8805(2) 0.0242(9) Uani 1 1 d . . .
N6 N 0.2443(5) 0.4763(4) 0.9742(3) 0.0476(13) Uani 1 1 d . . .
H6 H 0.1896 0.4427 1.0009 0.057 Uiso 1 1 calc R . .
C1 C 0.3389(5) 0.1650(4) 0.6937(3) 0.0226(10) Uani 1 1 d . . .
C2 C 0.2136(5) 0.1359(4) 0.6527(3) 0.0230(10) Uani 1 1 d . . .
C3 C 0.1434(4) 0.2260(4) 0.6592(3) 0.0226(10) Uani 1 1 d . . .
C4 C 0.1953(4) 0.3424(4) 0.7095(3) 0.0224(10) Uani 1 1 d . . .
C5 C 0.3202(4) 0.3698(4) 0.7506(2) 0.0200(10) Uani 1 1 d . . .
C6 C 0.3935(4) 0.2825(4) 0.7435(3) 0.0229(10) Uani 1 1 d . . .
C7 C 0.4172(5) 0.0717(4) 0.6837(3) 0.0316(12) Uani 1 1 d . . .
H7A H 0.3926 0.0210 0.6320 0.038 Uiso 1 1 calc R . .
H7B H 0.5083 0.1157 0.6902 0.038 Uiso 1 1 calc R . .
C8 C 0.1566(5) 0.0080(4) 0.6010(3) 0.0367(13) Uani 1 1 d . . .
H8A H 0.1940 0.0036 0.5547 0.055 Uiso 1 1 calc GR . .
H8B H 0.0644 -0.0066 0.5886 0.055 Uiso 1 1 calc GR . .
H8C H 0.1752 -0.0544 0.6269 0.055 Uiso 1 1 calc GR . .
C9 C 0.0132(4) 0.1986(4) 0.6105(3) 0.0283(11) Uani 1 1 d . . .
H9A H -0.0057 0.2768 0.6058 0.034 Uiso 1 1 calc R . .
H9B H 0.0165 0.1538 0.5595 0.034 Uiso 1 1 calc R . .
C10 C 0.1171(5) 0.4371(4) 0.7183(3) 0.0342(13) Uani 1 1 d . . .
H10A H 0.1261 0.4817 0.6778 0.051 Uiso 1 1 calc GR . .
H10B H 0.1481 0.4948 0.7669 0.051 Uiso 1 1 calc GR . .
H10C H 0.0274 0.3951 0.7159 0.051 Uiso 1 1 calc GR . .
C11 C 0.3775(5) 0.4987(4) 0.8024(3) 0.0280(11) Uani 1 1 d . . .
H11A H 0.4709 0.5210 0.8049 0.034 Uiso 1 1 calc R . .
H11B H 0.3446 0.5592 0.7801 0.034 Uiso 1 1 calc R . .
C12 C 0.5294(5) 0.3147(5) 0.7885(3) 0.0387(14) Uani 1 1 d . . .
H12A H 0.5438 0.2424 0.8051 0.058 Uiso 1 1 calc GR . .
H12B H 0.5383 0.3806 0.8325 0.058 Uiso 1 1 calc GR . .
H12C H 0.5918 0.3413 0.7565 0.058 Uiso 1 1 calc GR . .
C13 C 0.3678(5) 0.0168(5) 0.8082(3) 0.0371(14) Uani 1 1 d . . .
H13 H 0.3468 0.0897 0.8291 0.045 Uiso 1 1 calc R . .
C14 C 0.4071(6) -0.1646(5) 0.7954(3) 0.0411(15) Uani 1 1 d . . .
H14 H 0.4181 -0.2391 0.8062 0.049 Uiso 1 1 calc R . .
C15 C 0.4240(5) -0.1254(4) 0.7301(3) 0.0350(13) Uani 1 1 d . . .
H15 H 0.4480 -0.1680 0.6870 0.042 Uiso 1 1 calc R . .
C16 C -0.0817(6) 0.0739(6) 0.7022(3) 0.0506(17) Uani 1 1 d . . .
H16 H -0.0056 0.0852 0.7356 0.061 Uiso 1 1 calc R . .
C17 C -0.2844(5) 0.0108(5) 0.6488(3) 0.0399(14) Uani 1 1 d . . .
H17 H -0.3725 -0.0295 0.6392 0.048 Uiso 1 1 calc R . .
C18 C -0.2207(5) 0.0847(4) 0.6079(3) 0.0341(13) Uani 1 1 d . . .
H18 H -0.2559 0.1061 0.5643 0.041 Uiso 1 1 calc R . .
C19 C 0.2482(6) 0.4322(5) 0.9022(3) 0.0448(15) Uani 1 1 d . . .
H19 H 0.1909 0.3608 0.8712 0.054 Uiso 1 1 calc R . .
C20 C 0.4040(5) 0.6029(5) 0.9427(3) 0.0385(14) Uani 1 1 d . . .
H20 H 0.4746 0.6697 0.9438 0.046 Uiso 1 1 calc R . .
C21 C 0.3404(6) 0.5838(5) 1.0003(3) 0.0438(15) Uani 1 1 d . . .
H21 H 0.3580 0.6343 1.0493 0.053 Uiso 1 1 calc R . .
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'
Co Co 0.3494 0.9721 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Mo1 O3 100.22(14) . .
O1 Mo1 O6 87.81(14) . .
O1 Mo1 O9 100.76(14) . 2
O1 Mo1 O11 164.86(14) . 2
O2 Mo1 O1 105.35(17) . .
O2 Mo1 O3 99.79(14) . .
O2 Mo1 O6 165.87(14) . .
O2 Mo1 O9 102.65(14) . 2
O2 Mo1 O11 89.65(14) . 2
O3 Mo1 O6 72.27(11) . .
O3 Mo1 O11 78.76(11) . 2
O9 Mo1 O3 143.79(13) 2 .
O9 Mo1 O6 79.40(11) 2 .
O9 Mo1 O11 73.37(12) 2 2
O11 Mo1 O6 77.46(11) 2 .
O3 Mo2 O6 71.75(11) . .
O3 Mo2 O13 78.14(12) . 2
O4 Mo2 O3 100.48(14) . .
O4 Mo2 O6 164.28(14) . .
O4 Mo2 O7 102.36(15) . .
O4 Mo2 O13 88.18(14) . 2
O5 Mo2 O3 102.93(15) . .
O5 Mo2 O4 105.95(16) . .
O5 Mo2 O6 89.30(13) . .
O5 Mo2 O7 100.13(15) . .
O5 Mo2 O13 165.22(13) . 2
O7 Mo2 O3 141.43(12) . .
O7 Mo2 O6 78.09(11) . .
O7 Mo2 O13 71.99(12) . 2
O13 Mo2 O6 76.95(10) 2 .
O7 Mo3 O11 78.13(11) . .
O7 Mo3 O13 72.30(12) . 2
O8 Mo3 O7 103.36(14) . .
O8 Mo3 O9 100.57(14) . .
O8 Mo3 O11 165.46(14) . .
O8 Mo3 O13 89.66(14) . 2
O9 Mo3 O7 142.30(12) . .
O9 Mo3 O11 71.69(11) . .
O9 Mo3 O13 79.20(12) . 2
O10 Mo3 O7 100.52(15) . .
O10 Mo3 O8 105.38(16) . .
O10 Mo3 O9 100.68(15) . .
O10 Mo3 O11 88.38(13) . .
O10 Mo3 O13 164.63(13) . 2
O13 Mo3 O11 76.94(10) 2 .
O6 Mo4 O11 109.66(14) . .
O12 Mo4 O6 109.28(15) . .
O12 Mo4 O11 109.72(15) . .
O12 Mo4 O13 109.24(15) . .
O13 Mo4 O6 109.27(14) . .
O13 Mo4 O11 109.65(14) . .
Mo2 O3 Mo1 123.96(16) . .
Mo1 O6 Mo2 87.56(10) . .
Mo4 O6 Mo1 130.11(15) . .
Mo4 O6 Mo2 130.21(15) . .
Mo2 O7 Mo3 123.35(16) . .
Mo1 O9 Mo3 123.42(16) 2 .
Mo1 O11 Mo3 87.56(10) 2 .
Mo4 O11 Mo1 130.89(15) . 2
Mo4 O11 Mo3 129.83(15) . .
Mo3 O13 Mo2 87.11(10) 2 2
Mo4 O13 Mo2 130.02(15) . 2
Mo4 O13 Mo3 131.10(15) . 2
O14 Mo5 O16 100.52(13) . .
O14 Mo5 O17 161.10(12) . .
O14 Mo5 O19 91.64(12) . 2_666
O14 Mo5 O26 93.99(13) . .
O15 Mo5 O14 104.92(15) . .
O15 Mo5 O16 103.20(14) . .
O15 Mo5 O17 93.50(13) . .
O15 Mo5 O19 163.44(13) . 2_666
O15 Mo5 O26 103.52(14) . .
O16 Mo5 O17 78.87(11) . .
O16 Mo5 O19 73.56(11) . 2_666
O16 Mo5 O26 145.01(12) . .
O17 Mo5 O19 69.95(10) . 2_666
O26 Mo5 O17 77.34(11) . .
O26 Mo5 O19 74.37(11) . 2_666
O17 Mo6 Mo7 133.81(9) . .
O17 Mo6 O19 156.17(12) . .
O17 Mo6 O19 80.78(12) . 2_666
O17 Mo6 O20 97.46(12) . .
O17 Mo6 O23 96.10(12) . 2_666
O18 Mo6 Mo7 89.90(10) . .
O18 Mo6 O17 104.76(14) . .
O18 Mo6 O19 174.46(13) . 2_666
O18 Mo6 O19 99.06(13) . .
O18 Mo6 O20 100.67(13) . .
O18 Mo6 O23 101.32(13) . 2_666
O19 Mo6 Mo7 86.19(7) 2_666 .
O19 Mo6 Mo7 45.60(7) . .
O19 Mo6 O19 75.39(11) . 2_666
O20 Mo6 Mo7 36.36(8) . .
O20 Mo6 O19 78.41(11) . .
O20 Mo6 O19 78.42(10) . 2_666
O23 Mo6 Mo7 124.09(8) 2_666 .
O23 Mo6 O19 77.76(10) 2_666 2_666
O23 Mo6 O19 78.49(11) 2_666 .
O23 Mo6 O20 150.21(12) 2_666 .
O16 Mo7 Mo6 119.41(8) 2_666 .
O16 Mo7 O19 77.95(11) 2_666 .
O16 Mo7 O20 147.90(11) 2_666 .
O16 Mo7 O23 86.06(11) 2_666 .
O19 Mo7 Mo6 41.52(7) . .
O19 Mo7 O23 71.71(9) . .
O20 Mo7 Mo6 35.45(8) . .
O20 Mo7 O19 73.68(10) . .
O20 Mo7 O23 71.12(11) . .
O21 Mo7 Mo6 84.98(10) . .
O21 Mo7 O16 101.13(14) . 2_666
O21 Mo7 O19 95.01(13) . .
O21 Mo7 O20 96.04(14) . .
O21 Mo7 O23 163.44(12) . .
O22 Mo7 Mo6 135.58(11) . .
O22 Mo7 O16 101.35(14) . 2_666
O22 Mo7 O19 159.79(13) . .
O22 Mo7 O20 100.15(13) . .
O22 Mo7 O21 104.86(15) . .
O22 Mo7 O23 88.08(12) . .
O23 Mo7 Mo6 78.51(7) . .
O20 Mo8 O19 72.08(9) . 2_666
O23 Mo8 O19 72.79(10) . 2_666
O23 Mo8 O20 72.45(11) . .
O24 Mo8 O19 164.31(13) . 2_666
O24 Mo8 O20 92.27(12) . .
O24 Mo8 O23 102.05(13) . .
O24 Mo8 O25 105.27(14) . .
O24 Mo8 O26 101.06(14) . .
O25 Mo8 O19 90.30(12) . 2_666
O25 Mo8 O20 162.12(12) . .
O25 Mo8 O23 99.93(13) . .
O25 Mo8 O26 98.49(13) . .
O26 Mo8 O19 78.00(11) . 2_666
O26 Mo8 O20 81.17(11) . .
O26 Mo8 O23 145.33(12) . .
O14 Co1 O14 180.00(15) . 2_566
O25 Co1 O14 83.26(11) . .
O25 Co1 O14 96.74(11) 2_566 .
O25 Co1 O14 96.74(11) . 2_566
O25 Co1 O14 83.26(11) 2_566 2_566
O25 Co1 O25 180.0 . 2_566
O27 Co1 O14 92.33(13) . .
O27 Co1 O14 87.67(13) 2_566 .
O27 Co1 O14 87.67(13) . 2_566
O27 Co1 O14 92.33(13) 2_566 2_566
O27 Co1 O25 89.23(12) . .
O27 Co1 O25 89.23(12) 2_566 2_566
O27 Co1 O25 90.77(12) 2_566 .
O27 Co1 O25 90.77(12) . 2_566
O27 Co1 O27 180.0 . 2_566
Mo5 O14 Co1 144.24(16) . .
Mo7 O16 Mo5 118.22(15) 2_666 .
Mo6 O17 Mo5 118.78(15) . .
Mo6 O19 Mo5 90.38(10) 2_666 2_666
Mo6 O19 Mo5 164.91(14) . 2_666
Mo6 O19 Mo6 104.61(11) . 2_666
Mo6 O19 Mo7 92.88(10) . .
Mo6 O19 Mo8 91.94(10) . 2_666
Mo7 O19 Mo5 86.65(9) . 2_666
Mo7 O19 Mo6 98.10(10) . 2_666
Mo7 O19 Mo8 163.04(13) . 2_666
Mo8 O19 Mo5 84.50(9) 2_666 2_666
Mo8 O19 Mo6 96.39(10) 2_666 2_666
Mo6 O20 Mo7 108.19(13) . .
Mo6 O20 Mo8 110.25(12) . .
Mo7 O20 Mo8 104.12(12) . .
Mo6 O23 Mo7 109.16(12) 2_666 .
Mo6 O23 Mo8 110.59(13) 2_666 .
Mo8 O23 Mo7 103.68(12) . .
Mo8 O25 Co1 140.82(17) . .
Mo8 O26 Mo5 116.46(15) . .
Co1 O27 H27A 109.4 . .
Co1 O27 H27B 109.2 . .
H27A O27 H27B 109.1 . .
H30A O30 H30B 94.7 . .
H29A O29 H29B 100.8 . .
H28A O28 H28B 109.5 . .
C13 N1 C7 126.7(4) . .
C13 N1 C15 107.8(4) . .
C15 N1 C7 125.3(4) . .
C13 N2 H2 125.4 . .
C13 N2 C14 109.2(5) . .
C14 N2 H2 125.4 . .
C16 N3 C9 127.1(4) . .
C16 N3 C18 108.2(4) . .
C18 N3 C9 124.4(4) . .
C16 N4 H4 125.2 . .
C16 N4 C17 109.6(5) . .
C17 N4 H4 125.2 . .
C19 N5 C11 127.0(4) . .
C19 N5 C20 107.0(4) . .
C20 N5 C11 125.3(4) . .
C19 N6 H6 125.4 . .
C19 N6 C21 109.2(5) . .
C21 N6 H6 125.4 . .
C2 C1 C6 120.6(4) . .
C2 C1 C7 119.9(4) . .
C6 C1 C7 119.4(4) . .
C1 C2 C3 119.6(4) . .
C1 C2 C8 119.4(4) . .
C3 C2 C8 121.0(4) . .
C2 C3 C9 119.7(4) . .
C4 C3 C2 120.4(4) . .
C4 C3 C9 119.8(4) . .
C3 C4 C10 120.1(4) . .
C5 C4 C3 119.2(4) . .
C5 C4 C10 120.7(4) . .
C4 C5 C6 121.3(4) . .
C4 C5 C11 118.6(4) . .
C6 C5 C11 120.1(4) . .
C1 C6 C12 120.9(4) . .
C5 C6 C1 118.7(4) . .
C5 C6 C12 120.3(4) . .
N1 C7 C1 112.5(4) . .
N1 C7 H7A 109.1 . .
N1 C7 H7B 109.1 . .
C1 C7 H7A 109.1 . .
C1 C7 H7B 109.1 . .
H7A C7 H7B 107.8 . .
C2 C8 H8A 109.5 . .
C2 C8 H8B 109.5 . .
C2 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N3 C9 C3 113.0(4) . .
N3 C9 H9A 109.0 . .
N3 C9 H9B 109.0 . .
C3 C9 H9A 109.0 . .
C3 C9 H9B 109.0 . .
H9A C9 H9B 107.8 . .
C4 C10 H10A 109.5 . .
C4 C10 H10B 109.5 . .
C4 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N5 C11 C5 112.9(4) . .
N5 C11 H11A 109.0 . .
N5 C11 H11B 109.0 . .
C5 C11 H11A 109.0 . .
C5 C11 H11B 109.0 . .
H11A C11 H11B 107.8 . .
C6 C12 H12A 109.5 . .
C6 C12 H12B 109.5 . .
C6 C12 H12C 109.5 . .
H12A C12 H12B 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N1 C13 H13 125.6 . .
N2 C13 N1 108.9(4) . .
N2 C13 H13 125.6 . .
N2 C14 H14 126.4 . .
C15 C14 N2 107.1(4) . .
C15 C14 H14 126.4 . .
N1 C15 H15 126.5 . .
C14 C15 N1 107.0(5) . .
C14 C15 H15 126.5 . .
N3 C16 N4 108.1(5) . .
N3 C16 H16 125.9 . .
N4 C16 H16 125.9 . .
N4 C17 H17 126.5 . .
C18 C17 N4 107.0(5) . .
C18 C17 H17 126.5 . .
N3 C18 H18 126.5 . .
C17 C18 N3 107.1(5) . .
C17 C18 H18 126.5 . .
N5 C19 H19 125.5 . .
N6 C19 N5 109.0(5) . .
N6 C19 H19 125.5 . .
N5 C20 H20 126.1 . .
C21 C20 N5 107.8(5) . .
C21 C20 H20 126.1 . .
N6 C21 H21 126.5 . .
C20 C21 N6 106.9(5) . .
C20 C21 H21 126.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.704(3) .
Mo1 O2 1.691(3) .
Mo1 O3 1.917(3) .
Mo1 O6 2.429(3) .
Mo1 O9 1.906(3) 2
Mo1 O11 2.399(3) 2
Mo2 O3 1.910(3) .
Mo2 O4 1.711(3) .
Mo2 O5 1.702(3) .
Mo2 O6 2.455(3) .
Mo2 O7 1.895(3) .
Mo2 O13 2.448(3) 2
Mo3 O7 1.917(3) .
Mo3 O8 1.702(3) .
Mo3 O9 1.915(3) .
Mo3 O10 1.698(3) .
Mo3 O11 2.464(3) .
Mo3 O13 2.422(3) 2
Mo4 O6 1.791(3) .
Mo4 O11 1.793(3) .
Mo4 O12 1.707(3) .
Mo4 O13 1.784(3) .
O9 Mo1 1.906(3) 2
O11 Mo1 2.399(3) 2
O13 Mo2 2.448(3) 2
O13 Mo3 2.422(3) 2
Mo5 O14 1.739(3) .
Mo5 O15 1.689(3) .
Mo5 O16 1.911(3) .
Mo5 O17 2.229(3) .
Mo5 O19 2.476(3) 2_666
Mo5 O26 1.932(3) .
Mo6 Mo7 3.2151(5) .
Mo6 O17 1.750(3) .
Mo6 O18 1.694(3) .
Mo6 O19 2.134(3) .
Mo6 O19 2.361(3) 2_666
Mo6 O20 1.963(3) .
Mo6 O23 1.955(3) 2_666
Mo7 O16 1.911(3) 2_666
Mo7 O19 2.300(3) .
Mo7 O20 2.006(3) .
Mo7 O21 1.710(3) .
Mo7 O22 1.695(3) .
Mo7 O23 2.356(3) .
Mo8 O19 2.358(3) 2_666
Mo8 O20 2.318(3) .
Mo8 O23 1.978(3) .
Mo8 O24 1.692(3) .
Mo8 O25 1.734(3) .
Mo8 O26 1.893(3) .
Co1 O14 2.147(3) .
Co1 O14 2.147(3) 2_566
Co1 O25 2.129(3) .
Co1 O25 2.129(3) 2_566
Co1 O27 2.026(3) .
Co1 O27 2.026(3) 2_566
O16 Mo7 1.911(3) 2_666
O19 Mo5 2.476(3) 2_666
O19 Mo6 2.361(3) 2_666
O19 Mo8 2.358(3) 2_666
O23 Mo6 1.955(3) 2_666
O27 H27A 0.8544 .
O27 H27B 0.8543 .
O30 H30A 0.9665 .
O30 H30B 0.8860 .
O29 H29A 0.7812 .
O29 H29B 0.8503 .
O28 H28A 0.8502 .
O28 H28B 0.8500 .
N1 C7 1.481(6) .
N1 C13 1.321(6) .
N1 C15 1.372(5) .
N2 H2 0.8600 .
N2 C13 1.311(6) .
N2 C14 1.349(6) .
N3 C9 1.481(6) .
N3 C16 1.313(6) .
N3 C18 1.376(6) .
N4 H4 0.8600 .
N4 C16 1.315(7) .
N4 C17 1.349(7) .
N5 C11 1.469(6) .
N5 C19 1.322(6) .
N5 C20 1.384(6) .
N6 H6 0.8600 .
N6 C19 1.308(6) .
N6 C21 1.360(7) .
C1 C2 1.398(6) .
C1 C6 1.409(6) .
C1 C7 1.498(6) .
C2 C3 1.403(6) .
C2 C8 1.512(6) .
C3 C4 1.401(6) .
C3 C9 1.502(6) .
C4 C5 1.397(6) .
C4 C10 1.510(6) .
C5 C6 1.400(6) .
C5 C11 1.522(6) .
C6 C12 1.520(6) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13 0.9300 .
C14 H14 0.9300 .
C14 C15 1.342(7) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 H17 0.9300 .
C17 C18 1.329(7) .
C18 H18 0.9300 .
C19 H19 0.9300 .
C20 H20 0.9300 .
C20 C21 1.321(7) .
C21 H21 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O27 H27A O21 0.85 2.19 2.906(5) 140.8 1_455
O27 H27B O28 0.85 2.04 2.729(6) 137.9 .
O30 H30A O1 0.97 2.13 2.89(3) 134.6 1_656
O30 H30B O9 0.89 2.38 2.80(4) 109.0 1_556
O30 H30B O12 0.89 2.36 2.97(3) 125.9 2_556
O29 H29A O4 0.78 2.51 3.104(6) 133.8 .
O29 H29A O15 0.78 2.78 3.367(6) 134.2 .
O29 H29B O3 0.85 2.10 2.944(6) 171.1 2_565
O28 H28A O26 0.85 2.19 2.926(6) 145.1 .
O28 H28B O5 0.85 2.63 3.380(7) 147.7 .
O28 H28B O7 0.85 2.42 2.967(5) 122.8 .
N4 H4 O10 0.86 2.09 2.886(6) 153.9 2_556
N6 H6 O4 0.86 2.07 2.889(6) 159.3 1_556
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O3 Mo2 O7 Mo3 62.8(3) . .
O4 Mo2 O7 Mo3 -62.2(2) . .
O5 Mo2 O7 Mo3 -171.16(18) . .
O6 Mo2 O7 Mo3 101.72(18) . .
O6 Mo4 O11 Mo1 -125.1(2) . 2
O6 Mo4 O11 Mo3 5.4(3) . .
O6 Mo4 O13 Mo2 125.42(19) . 2
O6 Mo4 O13 Mo3 -4.8(2) . 2
O11 Mo4 O6 Mo1 124.25(19) . .
O11 Mo4 O6 Mo2 -5.5(2) . .
O11 Mo4 O13 Mo2 5.2(2) . 2
O11 Mo4 O13 Mo3 -125.0(2) . 2
O12 Mo4 O6 Mo1 -115.4(2) . .
O12 Mo4 O6 Mo2 114.8(2) . .
O12 Mo4 O11 Mo1 114.9(2) . 2
O12 Mo4 O11 Mo3 -114.7(2) . .
O12 Mo4 O13 Mo2 -115.1(2) . 2
O12 Mo4 O13 Mo3 114.7(2) . 2
O13 Mo2 O7 Mo3 21.74(15) 2 .
O13 Mo4 O6 Mo1 4.0(2) . .
O13 Mo4 O6 Mo2 -125.70(19) . .
O13 Mo4 O11 Mo1 -5.1(3) . 2
O13 Mo4 O11 Mo3 125.3(2) . .
Mo7 Mo6 O17 Mo5 72.63(17) . .
O15 Mo5 O14 Co1 121.2(3) . .
O16 Mo5 O14 Co1 -132.0(3) . .
O17 Mo5 O14 Co1 -45.6(6) . .
O18 Mo6 O17 Mo5 177.12(14) . .
O19 Mo5 O14 Co1 -58.4(3) 2_666 .
O19 Mo6 O17 Mo5 -2.95(13) 2_666 .
O19 Mo6 O17 Mo5 -4.2(4) . .
O19 Mo8 O25 Co1 73.2(2) 2_666 .
O19 Mo8 O26 Mo5 -23.79(14) 2_666 .
O20 Mo6 O17 Mo5 73.97(16) . .
O20 Mo8 O25 Co1 82.8(5) . .
O20 Mo8 O26 Mo5 -97.21(16) . .
O23 Mo6 O17 Mo5 -79.45(16) 2_666 .
O23 Mo8 O25 Co1 145.8(2) . .
O23 Mo8 O26 Mo5 -56.8(3) . .
O24 Mo8 O25 Co1 -108.7(3) . .
O24 Mo8 O26 Mo5 172.20(16) . .
O25 Mo8 O26 Mo5 64.71(18) . .
O26 Mo5 O14 Co1 16.0(3) . .
O26 Mo8 O25 Co1 -4.7(3) . .
N2 C14 C15 N1 0.7(6) . .
N4 C17 C18 N3 0.1(6) . .
N5 C20 C21 N6 -0.3(6) . .
C1 C2 C3 C4 -3.3(7) . .
C1 C2 C3 C9 175.1(4) . .
C2 C1 C6 C5 -0.5(7) . .
C2 C1 C6 C12 179.7(4) . .
C2 C1 C7 N1 -90.8(5) . .
C2 C3 C4 C5 2.8(7) . .
C2 C3 C4 C10 -177.8(4) . .
C2 C3 C9 N3 81.8(5) . .
C3 C4 C5 C6 -1.1(7) . .
C3 C4 C5 C11 177.4(4) . .
C4 C3 C9 N3 -99.8(5) . .
C4 C5 C6 C1 0.0(7) . .
C4 C5 C6 C12 179.8(4) . .
C4 C5 C11 N5 88.9(5) . .
C6 C1 C2 C3 2.2(7) . .
C6 C1 C2 C8 -178.6(4) . .
C6 C1 C7 N1 90.3(5) . .
C6 C5 C11 N5 -92.6(5) . .
C7 N1 C13 N2 -174.7(5) . .
C7 N1 C15 C14 174.3(5) . .
C7 C1 C2 C3 -176.7(4) . .
C7 C1 C2 C8 2.5(7) . .
C7 C1 C6 C5 178.4(4) . .
C7 C1 C6 C12 -1.4(7) . .
C8 C2 C3 C4 177.5(4) . .
C8 C2 C3 C9 -4.1(7) . .
C9 N3 C16 N4 -174.1(5) . .
C9 N3 C18 C17 174.3(4) . .
C9 C3 C4 C5 -175.6(4) . .
C9 C3 C4 C10 3.7(7) . .
C10 C4 C5 C6 179.5(4) . .
C10 C4 C5 C11 -2.0(6) . .
C11 N5 C19 N6 -172.5(5) . .
C11 N5 C20 C21 172.1(5) . .
C11 C5 C6 C1 -178.5(4) . .
C11 C5 C6 C12 1.3(6) . .
C13 N1 C7 C1 -27.7(7) . .
C13 N1 C15 C14 -0.2(6) . .
C13 N2 C14 C15 -0.9(7) . .
C14 N2 C13 N1 0.8(6) . .
C15 N1 C7 C1 158.9(4) . .
C15 N1 C13 N2 -0.4(6) . .
C16 N3 C9 C3 -5.6(7) . .
C16 N3 C18 C17 -0.2(6) . .
C16 N4 C17 C18 -0.1(7) . .
C17 N4 C16 N3 0.0(7) . .
C18 N3 C9 C3 -179.0(4) . .
C18 N3 C16 N4 0.1(7) . .
C19 N5 C11 C5 -23.3(7) . .
C19 N5 C20 C21 1.4(6) . .
C19 N6 C21 C20 -1.0(7) . .
C20 N5 C11 C5 167.8(4) . .
C20 N5 C19 N6 -2.0(6) . .
C21 N6 C19 N5 1.9(7) . .
