#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:33:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179146 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/07/4310767.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_4310767
loop_
_publ_author_name
'Cai-Ming Liu'
'Ebbe Nordlander'
'Derek Schmeh'
'Richard Shoemaker'
'Cortlandt G. Pierpont'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of Colorado
Boulder, CO  80309
;
_publ_contact_author_name        'Professor Cortlandt Pierpont'
_publ_section_title
;
 Coordination Complexes of Molybdenum with 3,6-Di-tert-butylcatechol.
 Addition Products of DMSO, Pyridine N-oxide, and Triphenylarsine Oxide to
 the Putative [MoVIO(3,6-DBCat)2] Monomer and Self-Assembly of the Chiral
 [{MoVIO(3,6-DBCat)2}4] Square
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2114
_journal_page_last               2124
_journal_paper_doi               10.1021/ic0354264
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C32 H52 Mo O7 S2'
_chemical_formula_weight         708.80
_chemical_name_systematic
; 
 MoO(dmso)(3,6-DBCat)2_DMSO 
;
_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
_cell_angle_alpha                99.5230(10)
_cell_angle_beta                 93.2470(10)
_cell_angle_gamma                114.6640(10)
_cell_formula_units_Z            2
_cell_length_a                   10.69460(10)
_cell_length_b                   11.23830(10)
_cell_length_c                   16.68450(10)
_cell_measurement_reflns_used    134
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      15.4
_cell_measurement_theta_min      10.1
_cell_volume                     1779.48(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      145(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19712
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        2.11
_diffrn_standards_interval_count 95
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.625
_refine_diff_density_min         -1.465
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0006(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.000
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_hydrogen_treatment    'fixed, riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_obs          0.0513
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0578P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1288
_refine_ls_wR_factor_obs         0.1090
_reflns_number_observed          6304
_reflns_number_total             8712
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0354264si20031211_050150_4.cif
_cod_data_source_block           MoO(dmso)(3,6-DBCat)2_DMSO
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1779.48(2)
_cod_database_code               4310767
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo Mo 0.22641(3) 0.02861(3) 0.15114(2) 0.01696(9) Uani 1 d . .
O1 O 0.3452(2) 0.1392(2) 0.25419(14) 0.0181(5) Uani 1 d . .
O2 O 0.3605(2) -0.0463(2) 0.15912(14) 0.0191(5) Uani 1 d . .
O3 O 0.0960(2) 0.0962(2) 0.19255(14) 0.0182(5) Uani 1 d . .
O4 O 0.1145(2) -0.1058(2) 0.22121(13) 0.0181(5) Uani 1 d . .
O5 O 0.2701(2) 0.1323(2) 0.08395(14) 0.0240(5) Uani 1 d . .
C1 C 0.4238(3) 0.0874(3) 0.2894(2) 0.0179(7) Uani 1 d . .
C2 C 0.4287(3) -0.0210(3) 0.2361(2) 0.0213(7) Uani 1 d . .
C3 C 0.4997(4) -0.0920(3) 0.2616(2) 0.0234(7) Uani 1 d . .
C4 C 0.5640(4) -0.0466(3) 0.3431(2) 0.0272(8) Uani 1 d . .
H4A H 0.6119(4) -0.0920(3) 0.3642(2) 0.033 Uiso 1 calc R .
C5 C 0.5605(4) 0.0632(3) 0.3950(2) 0.0265(8) Uani 1 d . .
H5B H 0.6068(4) 0.0896(3) 0.4496(2) 0.032 Uiso 1 calc R .
C6 C 0.4924(4) 0.1351(3) 0.3701(2) 0.0207(7) Uani 1 d . .
C7 C 0.5067(4) -0.2089(3) 0.2031(2) 0.0311(9) Uani 1 d . .
C8 C 0.5788(5) -0.2764(4) 0.2476(3) 0.0527(14) Uani 1 d . .
H8A H 0.5817(5) -0.3505(4) 0.2087(3) 0.079 Uiso 1 calc R .
H8B H 0.5272(5) -0.3110(4) 0.2918(3) 0.079 Uiso 1 calc R .
H8C H 0.6738(5) -0.2111(4) 0.2710(3) 0.079 Uiso 1 calc R .
C9 C 0.5914(4) -0.1530(4) 0.1357(3) 0.0370(10) Uani 1 d . .
H9A H 0.5465(4) -0.1092(4) 0.1064(3) 0.055 Uiso 1 calc R .
H9B H 0.5960(4) -0.2263(4) 0.0970(3) 0.055 Uiso 1 calc R .
H9C H 0.6856(4) -0.0877(4) 0.1605(3) 0.055 Uiso 1 calc R .
C10 C 0.3592(4) -0.3147(3) 0.1653(3) 0.0337(9) Uani 1 d . .
H10A H 0.3113(4) -0.2731(3) 0.1364(3) 0.050 Uiso 1 calc R .
H10B H 0.3074(4) -0.3510(3) 0.2090(3) 0.050 Uiso 1 calc R .
H10C H 0.3652(4) -0.3872(3) 0.1265(3) 0.050 Uiso 1 calc R .
C11 C 0.4871(4) 0.2546(3) 0.4276(2) 0.0234(7) Uani 1 d . .
C12 C 0.5289(4) 0.3746(3) 0.3854(2) 0.0316(9) Uani 1 d . .
H12A H 0.6236(4) 0.4002(3) 0.3721(2) 0.047 Uiso 1 calc R .
H12B H 0.5252(4) 0.4502(3) 0.4223(2) 0.047 Uiso 1 calc R .
H12C H 0.4646(4) 0.3500(3) 0.3348(2) 0.047 Uiso 1 calc R .
C13 C 0.3391(4) 0.2137(4) 0.4485(2) 0.0323(9) Uani 1 d . .
H13A H 0.3131(4) 0.1372(4) 0.4754(2) 0.048 Uiso 1 calc R .
H13B H 0.2745(4) 0.1888(4) 0.3980(2) 0.048 Uiso 1 calc R .
H13C H 0.3351(4) 0.2890(4) 0.4856(2) 0.048 Uiso 1 calc R .
C14 C 0.5886(4) 0.2989(4) 0.5076(2) 0.0343(9) Uani 1 d . .
H14A H 0.6835(4) 0.3252(4) 0.4946(2) 0.051 Uiso 1 calc R .
H14B H 0.5635(4) 0.2245(4) 0.5364(2) 0.051 Uiso 1 calc R .
H14C H 0.5833(4) 0.3751(4) 0.5428(2) 0.051 Uiso 1 calc R .
C15 C 0.0415(3) 0.0583(3) 0.2600(2) 0.0171(7) Uani 1 d . .
C16 C 0.0475(3) -0.0608(3) 0.2735(2) 0.0148(6) Uani 1 d . .
C17 C -0.0138(3) -0.1214(3) 0.3375(2) 0.0155(6) Uani 1 d . .
C18 C -0.0712(4) -0.0532(3) 0.3881(2) 0.0197(7) Uani 1 d . .
H18A H -0.1122(4) -0.0895(3) 0.4327(2) 0.024 Uiso 1 calc R .
C19 C -0.0711(4) 0.0676(3) 0.3759(2) 0.0212(7) Uani 1 d . .
H19A H -0.1112(4) 0.1099(3) 0.4133(2) 0.025 Uiso 1 calc R .
C20 C -0.0156(3) 0.1279(3) 0.3122(2) 0.0185(7) Uani 1 d . .
C21 C -0.0099(4) -0.2521(3) 0.3508(2) 0.0201(7) Uani 1 d . .
C22 C -0.1051(4) -0.3107(3) 0.4137(2) 0.0268(8) Uani 1 d . .
H22A H -0.2006(4) -0.3286(3) 0.3940(2) 0.040 Uiso 1 calc R .
H22B H -0.0733(4) -0.2466(3) 0.4664(2) 0.040 Uiso 1 calc R .
H22C H -0.1022(4) -0.3944(3) 0.4208(2) 0.040 Uiso 1 calc R .
C23 C 0.1392(4) -0.2241(3) 0.3816(2) 0.0284(8) Uani 1 d . .
H23A H 0.1723(4) -0.1573(3) 0.4332(2) 0.043 Uiso 1 calc R .
H23B H 0.1992(4) -0.1901(3) 0.3405(2) 0.043 Uiso 1 calc R .
H23C H 0.1415(4) -0.3071(3) 0.3908(2) 0.043 Uiso 1 calc R .
C24 C -0.0625(4) -0.3568(3) 0.2700(2) 0.0290(8) Uani 1 d . .
H24A H -0.1580(4) -0.3744(3) 0.2505(2) 0.044 Uiso 1 calc R .
H24B H -0.0603(4) -0.4399(3) 0.2791(2) 0.044 Uiso 1 calc R .
H24C H -0.0026(4) -0.3229(3) 0.2288(2) 0.044 Uiso 1 calc R .
C25 C -0.0158(4) 0.2595(3) 0.2989(2) 0.0241(8) Uani 1 d . .
C26 C 0.1316(4) 0.3619(3) 0.2945(3) 0.0332(9) Uani 1 d . .
H26A H 0.1296(4) 0.4453(3) 0.2860(3) 0.050 Uiso 1 calc R .
H26B H 0.1682(4) 0.3264(3) 0.2487(3) 0.050 Uiso 1 calc R .
H26C H 0.1913(4) 0.3795(3) 0.3459(3) 0.050 Uiso 1 calc R .
C27 C -0.0726(5) 0.3202(4) 0.3694(2) 0.0379(10) Uani 1 d . .
H27A H -0.1671(5) 0.2559(4) 0.3732(2) 0.057 Uiso 1 calc R .
H27B H -0.0741(5) 0.4027(4) 0.3585(2) 0.057 Uiso 1 calc R .
H27C H -0.0127(5) 0.3405(4) 0.4212(2) 0.057 Uiso 1 calc R .
C28 C -0.1113(4) 0.2296(3) 0.2188(2) 0.0283(8) Uani 1 d . .
H28A H -0.2051(4) 0.1640(3) 0.2225(2) 0.042 Uiso 1 calc R .
H28B H -0.0754(4) 0.1934(3) 0.1729(2) 0.042 Uiso 1 calc R .
H28C H -0.1143(4) 0.3124(3) 0.2097(2) 0.042 Uiso 1 calc R .
S1 S 0.00571(9) -0.27298(8) 0.06151(5) 0.0201(2) Uani 1 d . .
O6 O 0.1152(2) -0.1317(2) 0.05336(14) 0.0213(5) Uani 1 d . .
C29 C -0.0418(4) -0.3598(4) -0.0429(2) 0.0327(9) Uani 1 d . .
H29A H 0.0332(4) -0.3816(4) -0.0609(2) 0.049 Uiso 1 calc R .
H29B H -0.0577(4) -0.3030(4) -0.0771(2) 0.049 Uiso 1 calc R .
H29C H -0.1271(4) -0.4426(4) -0.0482(2) 0.049 Uiso 1 calc R .
C30 C -0.1457(4) -0.2483(3) 0.0756(2) 0.0261(8) Uani 1 d . .
H30A H -0.1361(4) -0.2002(3) 0.1319(2) 0.039 Uiso 1 calc R .
H30B H -0.2270(4) -0.3354(3) 0.0658(2) 0.039 Uiso 1 calc R .
H30C H -0.1576(4) -0.1958(3) 0.0369(2) 0.039 Uiso 1 calc R .
S2 S 0.62753(10) 0.34476(8) 0.06743(6) 0.0300(2) Uani 1 d . .
O7 O 0.7782(3) 0.4349(2) 0.0671(2) 0.0430(8) Uani 1 d . .
C31 C 0.5994(4) 0.3613(3) 0.1721(2) 0.0321(9) Uani 1 d . .
H31A H 0.6033(4) 0.4500(3) 0.1921(2) 0.048 Uiso 1 calc R .
H31B H 0.6715(4) 0.3508(3) 0.2050(2) 0.048 Uiso 1 calc R .
H31C H 0.5079(4) 0.2922(3) 0.1766(2) 0.048 Uiso 1 calc R .
C32 C 0.6140(4) 0.1783(3) 0.0516(2) 0.0295(8) Uani 1 d . .
H32A H 0.6272(4) 0.1510(3) -0.0049(2) 0.044 Uiso 1 calc R .
H32B H 0.5218(4) 0.1171(3) 0.0614(2) 0.044 Uiso 1 calc R .
H32C H 0.6854(4) 0.1757(3) 0.0898(2) 0.044 Uiso 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'
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
O5 Mo O2 109.21(11) . . ?
O5 Mo O3 91.89(10) . . ?
O2 Mo O3 155.11(9) . . ?
O5 Mo O1 104.13(10) . . ?
O2 Mo O1 78.39(9) . . ?
O3 Mo O1 83.86(9) . . ?
O5 Mo O4 163.03(10) . . ?
O2 Mo O4 85.70(9) . . ?
O3 Mo O4 75.83(8) . . ?
O1 Mo O4 86.41(9) . . ?
O5 Mo O6 89.16(10) . . ?
O2 Mo O6 87.08(9) . . ?
O3 Mo O6 106.84(9) . . ?
O1 Mo O6 162.84(9) . . ?
O4 Mo O6 83.40(8) . . ?
C1 O1 Mo 115.4(2) . . ?
C2 O2 Mo 115.1(2) . . ?
C15 O3 Mo 117.7(2) . . ?
C16 O4 Mo 114.5(2) . . ?
O1 C1 C6 124.3(3) . . ?
O1 C1 C2 112.9(3) . . ?
C6 C1 C2 122.8(3) . . ?
O2 C2 C3 125.1(3) . . ?
O2 C2 C1 113.0(3) . . ?
C3 C2 C1 121.8(3) . . ?
C4 C3 C2 115.0(3) . . ?
C4 C3 C7 123.2(3) . . ?
C2 C3 C7 121.8(3) . . ?
C3 C4 C5 122.5(3) . . ?
C6 C5 C4 123.0(3) . . ?
C5 C6 C1 114.8(3) . . ?
C5 C6 C11 122.9(3) . . ?
C1 C6 C11 122.3(3) . . ?
C8 C7 C3 111.4(3) . . ?
C8 C7 C9 108.4(4) . . ?
C3 C7 C9 108.0(3) . . ?
C8 C7 C10 108.3(3) . . ?
C3 C7 C10 110.2(3) . . ?
C9 C7 C10 110.5(3) . . ?
C13 C11 C12 109.9(3) . . ?
C13 C11 C6 109.0(3) . . ?
C12 C11 C6 110.0(3) . . ?
C13 C11 C14 109.1(3) . . ?
C12 C11 C14 107.6(3) . . ?
C6 C11 C14 111.3(3) . . ?
O3 C15 C20 124.3(3) . . ?
O3 C15 C16 112.8(3) . . ?
C20 C15 C16 122.9(3) . . ?
O4 C16 C17 125.2(3) . . ?
O4 C16 C15 113.8(3) . . ?
C17 C16 C15 121.0(3) . . ?
C18 C17 C16 115.7(3) . . ?
C18 C17 C21 123.3(3) . . ?
C16 C17 C21 120.9(3) . . ?
C17 C18 C19 122.5(3) . . ?
C20 C19 C18 123.3(3) . . ?
C19 C20 C15 114.4(3) . . ?
C19 C20 C25 123.3(3) . . ?
C15 C20 C25 122.3(3) . . ?
C23 C21 C24 109.7(3) . . ?
C23 C21 C22 109.5(3) . . ?
C24 C21 C22 107.5(3) . . ?
C23 C21 C17 109.4(3) . . ?
C24 C21 C17 110.0(3) . . ?
C22 C21 C17 110.7(3) . . ?
C26 C25 C20 110.5(3) . . ?
C26 C25 C28 110.5(3) . . ?
C20 C25 C28 108.2(3) . . ?
C26 C25 C27 108.3(3) . . ?
C20 C25 C27 111.2(3) . . ?
C28 C25 C27 108.2(3) . . ?
O6 S1 C30 103.19(15) . . ?
O6 S1 C29 101.31(15) . . ?
C30 S1 C29 99.0(2) . . ?
S1 O6 Mo 125.13(13) . . ?
O7 S2 C31 106.4(2) . . ?
O7 S2 C32 106.0(2) . . ?
C31 S2 C32 97.7(2) . . ?
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
Mo O5 1.694(2) . ?
Mo O2 1.951(2) . ?
Mo O3 1.954(2) . ?
Mo O1 1.960(2) . ?
Mo O4 2.077(2) . ?
Mo O6 2.084(2) . ?
O1 C1 1.363(4) . ?
O2 C2 1.365(4) . ?
O3 C15 1.347(4) . ?
O4 C16 1.326(4) . ?
C1 C6 1.401(5) . ?
C1 C2 1.406(4) . ?
C2 C3 1.405(5) . ?
C3 C4 1.398(5) . ?
C3 C7 1.534(5) . ?
C4 C5 1.400(5) . ?
C5 C6 1.386(5) . ?
C6 C11 1.539(5) . ?
C7 C8 1.527(5) . ?
C7 C9 1.534(6) . ?
C7 C10 1.541(5) . ?
C11 C13 1.532(5) . ?
C11 C12 1.537(5) . ?
C11 C14 1.541(5) . ?
C15 C20 1.406(4) . ?
C15 C16 1.420(4) . ?
C16 C17 1.407(4) . ?
C17 C18 1.383(4) . ?
C17 C21 1.538(4) . ?
C18 C19 1.405(4) . ?
C19 C20 1.385(5) . ?
C20 C25 1.532(4) . ?
C21 C23 1.530(5) . ?
C21 C24 1.535(5) . ?
C21 C22 1.537(5) . ?
C25 C26 1.530(5) . ?
C25 C28 1.534(5) . ?
C25 C27 1.542(5) . ?
S1 O6 1.565(2) . ?
S1 C30 1.775(4) . ?
S1 C29 1.780(4) . ?
S2 O7 1.504(3) . ?
S2 C31 1.781(4) . ?
S2 C32 1.788(3) . ?
