#------------------------------------------------------------------------------
#$Date: 2016-02-16 18:55:33 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176466 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/27/8102776.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_8102776
loop_
_publ_author_name
'Jiake Chen'
'Pingfan Wu'
'Zicheng Xiao'
'Jian Hao'
_publ_section_title
;
 Crystal structure of bis(tetrabutylammonium)
 oxopentathiocyanatomolybdate(V) --- ethanol (1:0.5),
 [(C4H9)4N]2[MoO(NCS)5] · 0.5C2H5OH
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              577
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         '2(C16 H36 N), 0.5(C2 H6 O), (C5 Mo N5 O S5)'
_chemical_formula_sum            'C38 H75 Mo N7 O1.5 S5'
_chemical_formula_weight         910.29
_chemical_name_systematic
;
Bis(tetrabutylammonium) Oxopentathiocyanatomolybdate(V)
;
_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                111.27(3)
_cell_angle_beta                 112.36(3)
_cell_angle_gamma                92.36(3)
_cell_formula_units_Z            4
_cell_length_a                   16.282(3)
_cell_length_b                   17.261(4)
_cell_length_c                   21.234(4)
_cell_measurement_reflns_used    64400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     5031(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37529
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         19666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0451P)²+2.3695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                13727
_reflns_number_total             19666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3075.cff
_cod_data_source_block           '[BuN4]2[MoO(NCS)5]'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C38 H75 Mo N7 O1.50 S5'
_cod_database_code               8102776
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 0.296921(16) 0.124008(14) 0.261769(13) 0.03978(7) Uani 1 1 d . . .
Mo2 Mo 0.145138(17) 0.420252(16) 0.696954(15) 0.04985(8) Uani 1 1 d . . .
S1 S 0.44565(6) 0.09979(5) 0.49637(4) 0.0594(2) Uani 1 1 d . . .
S2 S 0.37304(5) 0.42818(5) 0.39832(5) 0.0584(2) Uani 1 1 d . . .
S3 S 0.28590(7) -0.16780(5) 0.11566(6) 0.0759(3) Uani 1 1 d . . .
S4 S 0.20748(8) 0.17609(7) 0.03945(6) 0.0841(3) Uani 1 1 d . . .
S5 S 0.60407(5) 0.12855(5) 0.26103(5) 0.05238(19) Uani 1 1 d . . .
S6 S 0.22927(7) 0.72426(6) 0.81376(7) 0.0898(4) Uani 1 1 d . . .
S7 S -0.17654(6) 0.39314(7) 0.60733(6) 0.0841(3) Uani 1 1 d . . .
S8 S 0.09599(6) 0.12383(5) 0.65201(5) 0.0682(2) Uani 1 1 d . . .
S9 S 0.46262(6) 0.46297(7) 0.85178(6) 0.0807(3) Uani 1 1 d . . .
S10 S -0.00406(6) 0.39889(5) 0.84938(5) 0.0641(2) Uani 1 1 d . . .
O1 O 0.19367(13) 0.11079(13) 0.25973(12) 0.0586(5) Uani 1 1 d . . .
O2 O 0.15791(14) 0.40619(14) 0.61950(12) 0.0640(6) Uani 1 1 d . . .
N1 N 0.36237(16) 0.11256(13) 0.36032(13) 0.0447(5) Uani 1 1 d . . .
N2 N 0.33206(15) 0.25382(14) 0.31949(13) 0.0452(5) Uani 1 1 d . . .
N3 N 0.28818(16) -0.00265(14) 0.20296(13) 0.0482(6) Uani 1 1 d . . .
N4 N 0.25667(16) 0.14262(14) 0.16512(13) 0.0501(6) Uani 1 1 d . . .
N5 N 0.43366(16) 0.13603(13) 0.26257(12) 0.0418(5) Uani 1 1 d . . .
N6 N 0.16897(18) 0.55073(17) 0.74015(16) 0.0620(7) Uani 1 1 d . . .
N7 N 0.00759(18) 0.41332(17) 0.64803(15) 0.0613(7) Uani 1 1 d . . .
N8 N 0.12283(18) 0.29251(17) 0.67448(16) 0.0605(7) Uani 1 1 d . . .
N9 N 0.27785(18) 0.43225(16) 0.76574(15) 0.0576(7) Uani 1 1 d . . .
N10 N 0.11357(18) 0.43199(16) 0.79202(15) 0.0573(6) Uani 1 1 d . . .
N11 N -0.03498(15) 0.68340(14) 0.83655(13) 0.0462(6) Uani 1 1 d . . .
N12 N 0.19175(14) -0.11561(13) 0.34488(12) 0.0402(5) Uani 1 1 d . . .
N13 N 0.36805(14) 0.58970(12) 0.63974(12) 0.0374(5) Uani 1 1 d . . .
N14 N 0.37705(15) 0.18582(13) 0.85408(13) 0.0438(5) Uani 1 1 d . . .
C1 C 0.39864(19) 0.10843(16) 0.41801(17) 0.0428(6) Uani 1 1 d . . .
C2 C 0.34945(17) 0.32681(18) 0.35273(15) 0.0395(6) Uani 1 1 d . . .
C3 C 0.28803(19) -0.07124(18) 0.16608(16) 0.0473(7) Uani 1 1 d . . .
C4 C 0.2378(2) 0.15641(17) 0.11232(18) 0.0485(7) Uani 1 1 d . . .
C5 C 0.5040(2) 0.13188(15) 0.26122(14) 0.0395(6) Uani 1 1 d . . .
C6 C 0.1944(2) 0.6238(2) 0.77137(19) 0.0553(8) Uani 1 1 d . . .
C7 C -0.0693(2) 0.40570(19) 0.63140(17) 0.0546(8) Uani 1 1 d . . .
C8 C 0.11172(19) 0.2219(2) 0.66537(17) 0.0501(7) Uani 1 1 d . . .
C9 C 0.3556(2) 0.44534(19) 0.80267(18) 0.0540(8) Uani 1 1 d . . .
C10 C 0.0641(2) 0.41718(16) 0.81563(16) 0.0478(7) Uani 1 1 d . . .
C11 C 0.04164(19) 0.64790(18) 0.87759(16) 0.0462(7) Uani 1 1 d . . .
H11A H 0.0333 0.5886 0.8458 0.055 Uiso 1 1 calc R . .
H11B H 0.0984 0.6775 0.8844 0.055 Uiso 1 1 calc R . .
C12 C 0.0510(2) 0.6537(2) 0.95274(17) 0.0541(8) Uani 1 1 d . . .
H12A H -0.0020 0.6188 0.9467 0.065 Uiso 1 1 calc R . .
H12B H 0.0552 0.7120 0.9846 0.065 Uiso 1 1 calc R . .
C13 C 0.1358(2) 0.62326(18) 0.98841(16) 0.0521(7) Uani 1 1 d . . .
H13A H 0.1347 0.5681 0.9530 0.063 Uiso 1 1 calc R . .
H13B H 0.1887 0.6625 0.9994 0.063 Uiso 1 1 calc R . .
C14 C 0.1445(3) 0.6162(2) 1.05929(19) 0.0733(10) Uani 1 1 d . . .
H14A H 0.1991 0.5970 1.0794 0.110 Uiso 1 1 calc R . .
H14B H 0.0931 0.5764 1.0487 0.110 Uiso 1 1 calc R . .
H14C H 0.1469 0.6709 1.0950 0.110 Uiso 1 1 calc R . .
C15 C -0.0365(2) 0.6591(2) 0.75992(17) 0.0511(7) Uani 1 1 d . . .
H15A H 0.0222 0.6840 0.7664 0.061 Uiso 1 1 calc R . .
H15B H -0.0438 0.5978 0.7371 0.061 Uiso 1 1 calc R . .
C16 C -0.1088(2) 0.6849(2) 0.7063(2) 0.0647(9) Uani 1 1 d . . .
H16A H -0.1008 0.7463 0.7267 0.078 Uiso 1 1 calc R . .
H16B H -0.1683 0.6611 0.6992 0.078 Uiso 1 1 calc R . .
C17 C -0.1027(3) 0.6526(3) 0.6302(2) 0.0939(14) Uani 1 1 d . . .
H17A H -0.0438 0.6784 0.6379 0.113 Uiso 1 1 calc R . .
H17B H -0.1068 0.5916 0.6121 0.113 Uiso 1 1 calc R . .
C18 C -0.1738(3) 0.6709(3) 0.5722(2) 0.0956(13) Uani 1 1 d . . .
H18A H -0.1659 0.6488 0.5269 0.143 Uiso 1 1 calc R . .
H18B H -0.1691 0.7313 0.5888 0.143 Uiso 1 1 calc R . .
H18C H -0.2325 0.6446 0.5634 0.143 Uiso 1 1 calc R . .
C19 C -0.12552(19) 0.64559(17) 0.83030(17) 0.0497(7) Uani 1 1 d . . .
H19A H -0.1212 0.6600 0.8802 0.060 Uiso 1 1 calc R . .
H19B H -0.1720 0.6720 0.8064 0.060 Uiso 1 1 calc R . .
C20 C -0.1555(2) 0.55029(18) 0.78720(19) 0.0569(8) Uani 1 1 d . . .
H20A H -0.1027 0.5246 0.7972 0.068 Uiso 1 1 calc R . .
H20B H -0.1838 0.5368 0.7342 0.068 Uiso 1 1 calc R . .
C21 C -0.2220(2) 0.5128(2) 0.8079(2) 0.0722(10) Uani 1 1 d . . .
H21A H -0.2363 0.4515 0.7810 0.087 Uiso 1 1 calc R . .
H21B H -0.1928 0.5257 0.8608 0.087 Uiso 1 1 calc R . .
C22 C -0.3086(2) 0.5444(2) 0.7916(2) 0.0784(11) Uani 1 1 d . . .
H22A H -0.3467 0.5185 0.8068 0.118 Uiso 1 1 calc R . .
H22B H -0.3394 0.5299 0.7390 0.118 Uiso 1 1 calc R . .
H22C H -0.2954 0.6050 0.8185 0.118 Uiso 1 1 calc R . .
C23 C -0.0198(2) 0.77856(17) 0.8779(2) 0.0591(8) Uani 1 1 d . . .
H23A H -0.0201 0.7903 0.9261 0.071 Uiso 1 1 calc R . .
H23B H -0.0707 0.7980 0.8503 0.071 Uiso 1 1 calc R . .
C24 C 0.0670(3) 0.8304(2) 0.8907(3) 0.0925(14) Uani 1 1 d . B .
H24A H 0.0673 0.8213 0.8430 0.111 Uiso 1 1 calc R . .
H24B H 0.1188 0.8117 0.9182 0.111 Uiso 1 1 calc R . .
C25 C 0.0749(3) 0.9244(2) 0.9342(3) 0.0907(13) Uani 1 1 d . . .
H25C H 0.1337 0.9537 0.9458 0.109 Uiso 0.50 1 d PR A 1
H25D H 0.0727 0.9322 0.9806 0.109 Uiso 0.50 1 d PR A 1
H25A H 0.0205 0.9415 0.9098 0.109 Uiso 0.50 1 d PR . .
H25B H 0.1247 0.9562 0.9342 0.109 Uiso 0.50 1 d PR . .
C26A C 0.0900(6) 0.9437(5) 1.0081(5) 0.092(3) Uani 0.50 1 d P B .
H26A H 0.1365 0.9163 1.0292 0.139 Uiso 0.50 1 calc PR . .
H26B H 0.0349 0.9238 1.0093 0.139 Uiso 0.50 1 calc PR . .
H26C H 0.1090 1.0041 1.0365 0.139 Uiso 0.50 1 calc PR . .
C26B C 0.0125(8) 0.9628(7) 0.8994(6) 0.125(3) Uiso 0.50 1 d P B 1
H26D H 0.0070 0.9474 0.8495 0.187 Uiso 0.50 1 calc PR B 1
H26E H 0.0318 1.0234 0.9266 0.187 Uiso 0.50 1 calc PR B 1
H26F H -0.0452 0.9448 0.8976 0.187 Uiso 0.50 1 calc PR B 1
C27 C 0.10668(17) -0.15654(16) 0.27226(15) 0.0417(6) Uani 1 1 d . . .
H27A H 0.1000 -0.2178 0.2546 0.050 Uiso 1 1 calc R . .
H27B H 0.0548 -0.1422 0.2825 0.050 Uiso 1 1 calc R . .
C28 C 0.1040(2) -0.1316(2) 0.21013(17) 0.0551(8) Uani 1 1 d . . .
H28A H 0.1510 -0.1520 0.1949 0.066 Uiso 1 1 calc R . .
H28B H 0.1163 -0.0702 0.2284 0.066 Uiso 1 1 calc R . .
C29 C 0.0120(2) -0.1685(2) 0.14312(18) 0.0629(9) Uani 1 1 d . . .
H29A H 0.0155 -0.1583 0.1021 0.076 Uiso 1 1 calc R . .
H29B H -0.0018 -0.2296 0.1276 0.076 Uiso 1 1 calc R . .
C30 C -0.0640(3) -0.1322(4) 0.1580(2) 0.1140(17) Uani 1 1 d . . .
H30A H -0.1200 -0.1587 0.1140 0.171 Uiso 1 1 calc R . .
H30B H -0.0522 -0.0721 0.1715 0.171 Uiso 1 1 calc R . .
H30C H -0.0685 -0.1425 0.1982 0.171 Uiso 1 1 calc R . .
C31 C 0.18147(19) -0.15288(17) 0.39680(15) 0.0440(6) Uani 1 1 d . . .
H31A H 0.1737 -0.2141 0.3732 0.053 Uiso 1 1 calc R . .
H31B H 0.1264 -0.1411 0.4026 0.053 Uiso 1 1 calc R . .
C32 C 0.2598(2) -0.1204(2) 0.47384(17) 0.0589(8) Uani 1 1 d . . .
H32A H 0.2760 -0.0589 0.4945 0.071 Uiso 1 1 calc R . .
H32B H 0.3122 -0.1426 0.4699 0.071 Uiso 1 1 calc R . .
C33 C 0.2338(3) -0.1479(2) 0.52593(19) 0.0688(9) Uani 1 1 d . . .
H33A H 0.2095 -0.2086 0.5014 0.083 Uiso 1 1 calc R . .
H33B H 0.2883 -0.1370 0.5707 0.083 Uiso 1 1 calc R . .
C34 C 0.1655(3) -0.1035(3) 0.5479(2) 0.0930(13) Uani 1 1 d . . .
H34A H 0.1520 -0.1241 0.5800 0.139 Uiso 1 1 calc R . .
H34B H 0.1109 -0.1146 0.5040 0.139 Uiso 1 1 calc R . .
H34C H 0.1898 -0.0434 0.5739 0.139 Uiso 1 1 calc R . .
C35 C 0.20134(19) -0.01975(16) 0.37821(17) 0.0485(7) Uani 1 1 d . . .
H35A H 0.2580 0.0042 0.4230 0.058 Uiso 1 1 calc R . .
H35B H 0.2066 0.0013 0.3430 0.058 Uiso 1 1 calc R . .
C36 C 0.1264(2) 0.01410(17) 0.39830(18) 0.0537(7) Uani 1 1 d . . .
H36A H 0.0706 -0.0026 0.3533 0.064 Uiso 1 1 calc R . .
H36B H 0.1162 -0.0101 0.4300 0.064 Uiso 1 1 calc R . .
C37 C 0.1514(3) 0.1091(2) 0.4382(3) 0.0837(12) Uani 1 1 d . . .
H37A H 0.1615 0.1325 0.4059 0.100 Uiso 1 1 calc R . .
H37B H 0.2081 0.1249 0.4824 0.100 Uiso 1 1 calc R . .
C38 C 0.0806(3) 0.1484(2) 0.4614(2) 0.0805(11) Uani 1 1 d . . .
H38A H 0.1010 0.2090 0.4865 0.121 Uiso 1 1 calc R . .
H38B H 0.0713 0.1268 0.4945 0.121 Uiso 1 1 calc R . .
H38C H 0.0246 0.1343 0.4179 0.121 Uiso 1 1 calc R . .
C39 C 0.27667(18) -0.13137(17) 0.33325(16) 0.0461(7) Uani 1 1 d . . .
H39A H 0.2822 -0.1031 0.3026 0.055 Uiso 1 1 calc R . .
H39B H 0.3285 -0.1044 0.3814 0.055 Uiso 1 1 calc R . .
C40 C 0.28275(18) -0.22304(17) 0.29748(16) 0.0474(7) Uani 1 1 d . . .
H40A H 0.2326 -0.2512 0.2484 0.057 Uiso 1 1 calc R . .
H40B H 0.2792 -0.2526 0.3278 0.057 Uiso 1 1 calc R . .
C41 C 0.37263(19) -0.22552(19) 0.29064(17) 0.0532(7) Uani 1 1 d . . .
H41A H 0.3770 -0.1920 0.2635 0.064 Uiso 1 1 calc R . .
H41B H 0.4220 -0.1991 0.3403 0.064 Uiso 1 1 calc R . .
C42 C 0.3843(2) -0.3129(2) 0.2520(2) 0.0699(10) Uani 1 1 d . . .
H42A H 0.4421 -0.3095 0.2499 0.105 Uiso 1 1 calc R . .
H42B H 0.3368 -0.3390 0.2023 0.105 Uiso 1 1 calc R . .
H42C H 0.3816 -0.3462 0.2791 0.105 Uiso 1 1 calc R . .
C43 C 0.40230(19) 0.50758(16) 0.61711(16) 0.0447(7) Uani 1 1 d . . .
H43A H 0.3835 0.4840 0.5636 0.054 Uiso 1 1 calc R . .
H43B H 0.4681 0.5210 0.6409 0.054 Uiso 1 1 calc R . .
C44 C 0.3693(2) 0.44095(18) 0.63702(19) 0.0560(8) Uani 1 1 d . . .
H44A H 0.3035 0.4304 0.6166 0.067 Uiso 1 1 calc R . .
H44B H 0.3926 0.4622 0.6909 0.067 Uiso 1 1 calc R . .
C45 C 0.3986(2) 0.35834(19) 0.6078(2) 0.0603(8) Uani 1 1 d . . .
H45A H 0.4644 0.3681 0.6310 0.072 Uiso 1 1 calc R . .
H45B H 0.3792 0.3392 0.5544 0.072 Uiso 1 1 calc R . .
C46 C 0.3594(3) 0.2891(2) 0.6231(2) 0.0809(11) Uani 1 1 d . . .
H46A H 0.3798 0.2380 0.6037 0.121 Uiso 1 1 calc R . .
H46B H 0.2943 0.2784 0.5992 0.121 Uiso 1 1 calc R . .
H46C H 0.3795 0.3073 0.6759 0.121 Uiso 1 1 calc R . .
C47 C 0.41128(18) 0.65385(16) 0.62194(15) 0.0423(6) Uani 1 1 d . . .
H47A H 0.3895 0.7059 0.6374 0.051 Uiso 1 1 calc R . .
H47B H 0.4764 0.6670 0.6518 0.051 Uiso 1 1 calc R . .
C48 C 0.39417(18) 0.62726(17) 0.54175(15) 0.0435(6) Uani 1 1 d . . .
H48A H 0.3298 0.6048 0.5103 0.052 Uiso 1 1 calc R . .
H48B H 0.4262 0.5824 0.5282 0.052 Uiso 1 1 calc R . .
C49 C 0.4252(2) 0.70083(18) 0.52798(17) 0.0512(7) Uani 1 1 d . . .
H49A H 0.3900 0.7438 0.5384 0.061 Uiso 1 1 calc R . .
H49B H 0.4883 0.7259 0.5625 0.061 Uiso 1 1 calc R . .
C50 C 0.4160(2) 0.6764(2) 0.45031(19) 0.0727(10) Uani 1 1 d . . .
H50A H 0.4363 0.7259 0.4452 0.109 Uiso 1 1 calc R . .
H50B H 0.3536 0.6524 0.4157 0.109 Uiso 1 1 calc R . .
H50C H 0.4524 0.6353 0.4400 0.109 Uiso 1 1 calc R . .
C51 C 0.26564(18) 0.56984(17) 0.59769(17) 0.0470(7) Uani 1 1 d . . .
H51A H 0.2500 0.5344 0.5457 0.056 Uiso 1 1 calc R . .
H51B H 0.2406 0.5363 0.6167 0.056 Uiso 1 1 calc R . .
C52 C 0.21917(19) 0.64368(18) 0.60064(18) 0.0517(7) Uani 1 1 d . . .
H52A H 0.2375 0.6746 0.5764 0.062 Uiso 1 1 calc R . .
H52B H 0.2367 0.6822 0.6522 0.062 Uiso 1 1 calc R . .
C53 C 0.1161(2) 0.6110(2) 0.56120(19) 0.0581(8) Uani 1 1 d . . .
H53A H 0.1002 0.5673 0.5117 0.070 Uiso 1 1 calc R . .
H53B H 0.0978 0.5854 0.5888 0.070 Uiso 1 1 calc R . .
C54 C 0.0649(2) 0.6808(2) 0.5543(2) 0.0728(10) Uani 1 1 d . . .
H54A H 0.0008 0.6573 0.5287 0.109 Uiso 1 1 calc R . .
H54B H 0.0825 0.7062 0.5268 0.109 Uiso 1 1 calc R . .
H54C H 0.0788 0.7233 0.6032 0.109 Uiso 1 1 calc R . .
C55 C 0.3938(2) 0.62889(18) 0.72411(16) 0.0508(7) Uani 1 1 d . . .
H55A H 0.3771 0.6839 0.7371 0.061 Uiso 1 1 calc R . .
H55B H 0.3579 0.5930 0.7345 0.061 Uiso 1 1 calc R . .
C56 C 0.4927(2) 0.6405(2) 0.77418(17) 0.0672(9) Uani 1 1 d . . .
H56A H 0.5295 0.6731 0.7619 0.081 Uiso 1 1 calc R . .
H56B H 0.5088 0.5853 0.7647 0.081 Uiso 1 1 calc R . .
C57 C 0.5145(3) 0.6857(2) 0.85673(19) 0.0793(11) Uani 1 1 d . . .
H57A H 0.4705 0.6587 0.8669 0.095 Uiso 1 1 calc R . .
H57B H 0.5739 0.6786 0.8858 0.095 Uiso 1 1 calc R . .
C58 C 0.5141(3) 0.7763(2) 0.8814(2) 0.0928(13) Uani 1 1 d . . .
H58A H 0.5268 0.8003 0.9335 0.139 Uiso 1 1 calc R . .
H58B H 0.4555 0.7841 0.8531 0.139 Uiso 1 1 calc R . .
H58C H 0.5596 0.8042 0.8740 0.139 Uiso 1 1 calc R . .
C59 C 0.34156(19) 0.10560(17) 0.85805(16) 0.0480(7) Uani 1 1 d . . .
H59A H 0.3884 0.0723 0.8626 0.058 Uiso 1 1 calc R . .
H59B H 0.3326 0.1223 0.9034 0.058 Uiso 1 1 calc R . .
C60 C 0.2549(2) 0.04899(18) 0.79395(17) 0.0530(7) Uani 1 1 d . . .
H60A H 0.2646 0.0252 0.7490 0.064 Uiso 1 1 calc R . .
H60B H 0.2083 0.0820 0.7855 0.064 Uiso 1 1 calc R . .
C61 C 0.2239(2) -0.02236(19) 0.81085(19) 0.0609(8) Uani 1 1 d . . .
H61A H 0.2729 -0.0522 0.8232 0.073 Uiso 1 1 calc R . .
H61B H 0.2109 0.0019 0.8541 0.073 Uiso 1 1 calc R . .
C62 C 0.1404(3) -0.0853(2) 0.7462(2) 0.0913(13) Uani 1 1 d . . .
H62A H 0.1232 -0.1285 0.7599 0.137 Uiso 1 1 calc R . .
H62B H 0.1534 -0.1111 0.7036 0.137 Uiso 1 1 calc R . .
H62C H 0.0915 -0.0563 0.7340 0.137 Uiso 1 1 calc R . .
C63 C 0.3141(2) 0.24843(17) 0.86064(16) 0.0483(7) Uani 1 1 d . . .
H63A H 0.3336 0.2942 0.8499 0.058 Uiso 1 1 calc R . .
H63B H 0.2534 0.2194 0.8223 0.058 Uiso 1 1 calc R . .
C64 C 0.3086(2) 0.2874(2) 0.93487(18) 0.0585(8) Uani 1 1 d . . .
H64A H 0.3677 0.3203 0.9739 0.070 Uiso 1 1 calc R . .
H64B H 0.2899 0.2430 0.9474 0.070 Uiso 1 1 calc R . .
C65 C 0.2395(3) 0.3450(2) 0.92892(19) 0.0682(9) Uani 1 1 d . . .
H65A H 0.2578 0.3878 0.9146 0.082 Uiso 1 1 calc R . .
H65B H 0.1807 0.3112 0.8900 0.082 Uiso 1 1 calc R . .
C66 C 0.2306(3) 0.3885(3) 1.0011(2) 0.0967(14) Uani 1 1 d . . .
H66A H 0.1862 0.4233 0.9945 0.145 Uiso 1 1 calc R . .
H66B H 0.2882 0.4235 1.0395 0.145 Uiso 1 1 calc R . .
H66C H 0.2118 0.3465 1.0153 0.145 Uiso 1 1 calc R . .
C67 C 0.3792(2) 0.16668(17) 0.77919(16) 0.0458(7) Uani 1 1 d . . .
H67A H 0.3174 0.1452 0.7408 0.055 Uiso 1 1 calc R . .
H67B H 0.4016 0.2197 0.7793 0.055 Uiso 1 1 calc R . .
C68 C 0.4361(2) 0.10389(18) 0.75735(16) 0.0487(7) Uani 1 1 d . . .
H68A H 0.4191 0.0521 0.7616 0.058 Uiso 1 1 calc R . .
H68B H 0.4998 0.1278 0.7907 0.058 Uiso 1 1 calc R . .
C69 C 0.4215(2) 0.08371(19) 0.67768(17) 0.0525(7) Uani 1 1 d . . .
H69A H 0.3573 0.0618 0.6451 0.063 Uiso 1 1 calc R . .
H69B H 0.4395 0.1357 0.6742 0.063 Uiso 1 1 calc R . .
C70 C 0.4744(2) 0.01946(19) 0.65100(18) 0.0587(8) Uani 1 1 d . . .
H70A H 0.4624 0.0087 0.6004 0.088 Uiso 1 1 calc R . .
H70B H 0.4563 -0.0325 0.6536 0.088 Uiso 1 1 calc R . .
H70C H 0.5382 0.0414 0.6822 0.088 Uiso 1 1 calc R . .
C71 C 0.47124(19) 0.22267(18) 0.91789(16) 0.0509(7) Uani 1 1 d . . .
H71A H 0.4663 0.2305 0.9638 0.061 Uiso 1 1 calc R . .
H71B H 0.5087 0.1811 0.9102 0.061 Uiso 1 1 calc R . .
C72 C 0.5198(2) 0.30569(19) 0.92854(18) 0.0571(8) Uani 1 1 d . . .
H72A H 0.4804 0.3463 0.9300 0.069 Uiso 1 1 calc R . .
H72B H 0.5348 0.2971 0.8867 0.069 Uiso 1 1 calc R . .
C73 C 0.6072(2) 0.3413(2) 1.00143(19) 0.0640(9) Uani 1 1 d . . .
H73A H 0.5922 0.3471 1.0428 0.077 Uiso 1 1 calc R . .
H73B H 0.6474 0.3015 0.9989 0.077 Uiso 1 1 calc R . .
C74 C 0.6555(2) 0.4265(2) 1.0156(2) 0.0822(11) Uani 1 1 d . . .
H74A H 0.7094 0.4468 1.0617 0.123 Uiso 1 1 calc R . .
H74B H 0.6162 0.4662 1.0188 0.123 Uiso 1 1 calc R . .
H74C H 0.6718 0.4207 0.9754 0.123 Uiso 1 1 calc R . .
O3 O 0.4953(4) 0.0062(4) 0.0761(3) 0.0845(16) Uani 0.50 1 d P C 1
H3 H 0.5190 0.0568 0.1013 0.127 Uiso 0.50 1 calc PR C 1
C75 C 0.3821(17) -0.0069(14) 0.0483(17) 0.143(15) Uani 0.50 1 d P C 1
H75A H 0.3632 -0.0129 0.0848 0.171 Uiso 0.50 1 calc PR C 1
H75B H 0.3572 0.0373 0.0338 0.171 Uiso 0.50 1 calc PR C 1
C76 C 0.3630(9) -0.0874(7) -0.0155(9) 0.094(4) Uani 0.50 1 d P C 1
H76A H 0.2985 -0.1080 -0.0431 0.142 Uiso 0.50 1 calc PR C 1
H76B H 0.3898 -0.1284 0.0021 0.142 Uiso 0.50 1 calc PR C 1
H76C H 0.3881 -0.0788 -0.0472 0.142 Uiso 0.50 1 calc PR C 1
O4 O 0.4795(5) -0.0679(6) 0.0270(5) 0.117(2) Uani 0.50 1 d P D 2
H4 H 0.4959 -0.0433 0.0060 0.175 Uiso 0.50 1 calc PR D 2
C77 C 0.4182(10) -0.0215(10) 0.0573(11) 0.074(4) Uani 0.50 1 d P D 2
H77A H 0.4136 -0.0376 0.0953 0.089 Uiso 0.50 1 calc PR D 2
H77B H 0.4403 0.0395 0.0787 0.089 Uiso 0.50 1 calc PR D 2
C78 C 0.3383(14) -0.0448(18) -0.0015(12) 0.207(15) Uani 0.50 1 d P D 2
H78A H 0.2945 -0.0183 0.0139 0.310 Uiso 0.50 1 calc PR D 2
H78B H 0.3186 -0.1055 -0.0229 0.310 Uiso 0.50 1 calc PR D 2
H78C H 0.3441 -0.0275 -0.0381 0.310 Uiso 0.50 1 calc PR D 2
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'
S S 0.1246 0.1234 '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
O1 Mo1 N1 95.29(10) . . ?
O1 Mo1 N4 95.95(11) . . ?
N1 Mo1 N4 168.63(9) . . ?
O1 Mo1 N3 95.01(10) . . ?
N1 Mo1 N3 90.66(10) . . ?
N4 Mo1 N3 90.11(10) . . ?
O1 Mo1 N2 97.30(10) . . ?
N1 Mo1 N2 89.01(10) . . ?
N4 Mo1 N2 87.82(10) . . ?
N3 Mo1 N2 167.66(9) . . ?
O1 Mo1 N5 177.73(9) . . ?
N1 Mo1 N5 84.43(9) . . ?
N4 Mo1 N5 84.41(9) . . ?
N3 Mo1 N5 82.74(9) . . ?
N2 Mo1 N5 84.95(9) . . ?
O2 Mo2 N9 98.33(11) . . ?
O2 Mo2 N6 96.62(11) . . ?
N9 Mo2 N6 87.16(11) . . ?
O2 Mo2 N7 93.87(11) . . ?
N9 Mo2 N7 167.78(11) . . ?
N6 Mo2 N7 90.79(11) . . ?
O2 Mo2 N8 94.79(11) . . ?
N9 Mo2 N8 89.19(11) . . ?
N6 Mo2 N8 168.41(11) . . ?
N7 Mo2 N8 90.46(11) . . ?
O2 Mo2 N10 174.11(10) . . ?
N9 Mo2 N10 87.04(10) . . ?
N6 Mo2 N10 85.99(11) . . ?
N7 Mo2 N10 80.79(11) . . ?
N8 Mo2 N10 82.83(10) . . ?
C1 N1 Mo1 177.5(2) . . ?
C2 N2 Mo1 177.7(2) . . ?
C3 N3 Mo1 172.7(2) . . ?
C4 N4 Mo1 176.6(2) . . ?
C5 N5 Mo1 171.7(2) . . ?
C6 N6 Mo2 170.2(3) . . ?
C7 N7 Mo2 167.1(3) . . ?
C8 N8 Mo2 176.8(3) . . ?
C9 N9 Mo2 173.1(2) . . ?
C10 N10 Mo2 150.9(2) . . ?
C23 N11 C15 111.9(2) . . ?
C23 N11 C11 111.3(2) . . ?
C15 N11 C11 105.59(19) . . ?
C23 N11 C19 106.49(19) . . ?
C15 N11 C19 110.7(2) . . ?
C11 N11 C19 111.0(2) . . ?
C39 N12 C27 111.8(2) . . ?
C39 N12 C31 111.4(2) . . ?
C27 N12 C31 106.40(19) . . ?
C39 N12 C35 106.19(19) . . ?
C27 N12 C35 110.5(2) . . ?
C31 N12 C35 110.6(2) . . ?
C51 N13 C47 110.9(2) . . ?
C51 N13 C43 108.7(2) . . ?
C47 N13 C43 109.48(19) . . ?
C51 N13 C55 109.0(2) . . ?
C47 N13 C55 107.9(2) . . ?
C43 N13 C55 111.0(2) . . ?
C67 N14 C71 111.7(2) . . ?
C67 N14 C59 111.4(2) . . ?
C71 N14 C59 106.1(2) . . ?
C67 N14 C63 105.3(2) . . ?
C71 N14 C63 111.6(2) . . ?
C59 N14 C63 110.8(2) . . ?
N1 C1 S1 177.9(3) . . ?
N2 C2 S2 179.6(3) . . ?
N3 C3 S3 178.3(3) . . ?
N4 C4 S4 177.5(3) . . ?
N5 C5 S5 178.5(3) . . ?
N6 C6 S6 179.6(3) . . ?
N7 C7 S7 178.9(3) . . ?
N8 C8 S8 179.5(3) . . ?
N9 C9 S9 178.8(3) . . ?
N10 C10 S10 178.7(3) . . ?
C12 C11 N11 116.7(2) . . ?
C11 C12 C13 109.3(2) . . ?
C14 C13 C12 113.1(3) . . ?
C16 C15 N11 116.7(2) . . ?
C15 C16 C17 109.9(3) . . ?
C18 C17 C16 114.3(3) . . ?
C20 C19 N11 114.8(2) . . ?
C19 C20 C21 112.0(3) . . ?
C22 C21 C20 114.3(3) . . ?
N11 C23 C24 116.1(2) . . ?
C23 C24 C25 110.8(3) . . ?
C26B C25 C26A 114.6(7) . . ?
C26B C25 C24 116.8(6) . . ?
C26A C25 C24 112.2(5) . . ?
C28 C27 N12 115.7(2) . . ?
C27 C28 C29 111.2(2) . . ?
C30 C29 C28 113.7(3) . . ?
N12 C31 C32 115.6(2) . . ?
C31 C32 C33 110.7(3) . . ?
C34 C33 C32 114.0(3) . . ?
C36 C35 N12 117.3(2) . . ?
C37 C36 C35 110.4(2) . . ?
C36 C37 C38 114.0(3) . . ?
C40 C39 N12 117.0(2) . . ?
C39 C40 C41 109.0(2) . . ?
C42 C41 C40 114.1(3) . . ?
C44 C43 N13 114.5(2) . . ?
C43 C44 C45 112.4(2) . . ?
C44 C45 C46 112.3(3) . . ?
C48 C47 N13 116.1(2) . . ?
C47 C48 C49 111.5(2) . . ?
C50 C49 C48 113.7(3) . . ?
C52 C51 N13 117.4(2) . . ?
C51 C52 C53 109.5(2) . . ?
C54 C53 C52 112.5(3) . . ?
C56 C55 N13 115.7(2) . . ?
C55 C56 C57 112.8(3) . . ?
C58 C57 C56 114.0(3) . . ?
C60 C59 N14 117.1(2) . . ?
C59 C60 C61 110.1(3) . . ?
C62 C61 C60 112.8(3) . . ?
C64 C63 N14 116.7(2) . . ?
C63 C64 C65 108.6(2) . . ?
C66 C65 C64 112.6(3) . . ?
C68 C67 N14 116.6(2) . . ?
C67 C68 C69 109.7(2) . . ?
C70 C69 C68 112.9(2) . . ?
C72 C71 N14 116.6(2) . . ?
C71 C72 C73 110.5(3) . . ?
C74 C73 C72 111.9(3) . . ?
C76 C75 O3 93.4(12) . . ?
C78 C77 O4 104.7(16) . . ?
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 O1 1.669(2) . ?
Mo1 N1 2.043(3) . ?
Mo1 N4 2.054(3) . ?
Mo1 N3 2.054(2) . ?
Mo1 N2 2.054(2) . ?
Mo1 N5 2.220(2) . ?
Mo2 O2 1.668(2) . ?
Mo2 N9 2.046(3) . ?
Mo2 N6 2.055(3) . ?
Mo2 N7 2.056(3) . ?
Mo2 N8 2.064(3) . ?
Mo2 N10 2.209(3) . ?
S1 C1 1.611(3) . ?
S2 C2 1.606(3) . ?
S3 C3 1.612(3) . ?
S4 C4 1.602(3) . ?
S5 C5 1.635(3) . ?
S6 C6 1.593(4) . ?
S7 C7 1.602(4) . ?
S8 C8 1.604(3) . ?
S9 C9 1.600(4) . ?
S10 C10 1.608(3) . ?
N1 C1 1.171(3) . ?
N2 C2 1.157(3) . ?
N3 C3 1.158(3) . ?
N4 C4 1.160(4) . ?
N5 C5 1.160(3) . ?
N6 C6 1.159(4) . ?
N7 C7 1.152(4) . ?
N8 C8 1.157(4) . ?
N9 C9 1.166(4) . ?
N10 C10 1.161(4) . ?
N11 C23 1.512(3) . ?
N11 C15 1.516(4) . ?
N11 C11 1.521(4) . ?
N11 C19 1.525(3) . ?
N12 C39 1.513(3) . ?
N12 C27 1.516(3) . ?
N12 C31 1.518(3) . ?
N12 C35 1.519(3) . ?
N13 C51 1.514(3) . ?
N13 C47 1.519(3) . ?
N13 C43 1.525(3) . ?
N13 C55 1.539(3) . ?
N14 C67 1.517(3) . ?
N14 C71 1.518(4) . ?
N14 C59 1.521(3) . ?
N14 C63 1.526(3) . ?
C11 C12 1.509(4) . ?
C12 C13 1.519(4) . ?
C13 C14 1.507(4) . ?
C15 C16 1.508(4) . ?
C16 C17 1.550(5) . ?
C17 C18 1.477(5) . ?
C19 C20 1.511(4) . ?
C20 C21 1.515(4) . ?
C21 C22 1.495(5) . ?
C23 C24 1.516(4) . ?
C24 C25 1.518(5) . ?
C25 C26B 1.363(11) . ?
C25 C26A 1.398(9) . ?
C27 C28 1.516(4) . ?
C28 C29 1.522(4) . ?
C29 C30 1.497(5) . ?
C31 C32 1.518(4) . ?
C32 C33 1.531(4) . ?
C33 C34 1.500(5) . ?
C35 C36 1.511(4) . ?
C36 C37 1.498(4) . ?
C37 C38 1.512(5) . ?
C39 C40 1.513(4) . ?
C40 C41 1.526(4) . ?
C41 C42 1.492(4) . ?
C43 C44 1.505(4) . ?
C44 C45 1.512(4) . ?
C45 C46 1.523(5) . ?
C47 C48 1.500(4) . ?
C48 C49 1.511(4) . ?
C49 C50 1.491(4) . ?
C51 C52 1.503(4) . ?
C52 C53 1.531(4) . ?
C53 C54 1.512(4) . ?
C55 C56 1.510(4) . ?
C56 C57 1.523(5) . ?
C57 C58 1.459(5) . ?
C59 C60 1.502(4) . ?
C60 C61 1.519(4) . ?
C61 C62 1.514(5) . ?
C63 C64 1.513(4) . ?
C64 C65 1.532(4) . ?
C65 C66 1.509(5) . ?
C67 C68 1.514(4) . ?
C68 C69 1.516(4) . ?
C69 C70 1.513(4) . ?
C71 C72 1.505(4) . ?
C72 C73 1.536(4) . ?
C73 C74 1.509(5) . ?
O3 C75 1.69(2) . ?
C75 C76 1.46(3) . ?
O4 C77 1.494(15) . ?
C77 C78 1.33(3) . ?
