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#$Date: 2016-03-23 21:24:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179448 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/45/4334523.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_4334523
loop_
_publ_author_name
'Brian S. Dolinar'
'John F. Berry'
_publ_contact_author_address
;
1101 University Avenue
Madison, WI 53706
USA
;
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John Berry'
_publ_section_title
;
 Lewis Acid Enhanced Axial Ligation of [Mo2]4+ Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4658
_journal_page_last               4667
_journal_paper_doi               10.1021/ic400275x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C16 H16 Mo2 N4 O4 S4'
_chemical_formula_sum            'C16 H16 Mo2 N4 O4 S4'
_chemical_formula_weight         648.45
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6032(7)
_cell_length_b                   12.5912(10)
_cell_length_c                   15.8418(15)
_cell_measurement_reflns_used    9457
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      71.602
_cell_measurement_theta_min      5.455
_cell_volume                     2115.0(3)
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60° ω and 0.6° φ scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30667
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         72.03
_diffrn_reflns_theta_min         5.45
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.700
_exptl_absorpt_correction_T_max  0.4949
_exptl_absorpt_correction_T_min  0.0813
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
? was used for absorption correction.
wR2(int) was 0.1008 before and 0.0460 after correction.
The Ratio of minimum to maximum transmission is 0.1643.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'orange red'
_exptl_crystal_colour_modifier   orange
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.344
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0271
_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)+(0.0430P)²+3.0934P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                1958
_reflns_number_total             2040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400275x_si_001_2.cif
_cod_data_source_block           compound1a
_cod_database_code               4334523
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y+1/2, z'
3 '-x, y+1/2, -z+1/2'
4 'x+1/2, -y, -z+1/2'
5 '-x, -y, -z'
6 'x-1/2, y-1/2, -z'
7 'x, -y-1/2, z-1/2'
8 '-x-1/2, y, z-1/2'
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
Mo1 Mo 0.17583(2) 0.305918(16) 0.097204(14) 0.02050(11) Uani 1 1 d .
S1 S 0.44962(7) 0.28011(6) -0.01544(5) 0.03034(18) Uani 1 1 d .
S2 S 0.26108(7) 0.42580(5) 0.20712(4) 0.02616(17) Uani 1 1 d .
O1 O 0.1242(2) 0.5543(2) 0.01991(16) 0.0444(6) Uani 1 1 d .
O2 O 0.5937(2) 0.15604(18) 0.20745(15) 0.0355(5) Uani 1 1 d .
N1 N 0.2579(2) 0.41016(19) 0.00582(15) 0.0262(5) Uani 1 1 d .
N2 N 0.4315(2) 0.27438(18) 0.19319(14) 0.0213(5) Uani 1 1 d .
C1 C 0.3648(3) 0.3900(3) -0.03409(18) 0.0287(6) Uani 1 1 d .
C2 C 0.4019(3) 0.4768(3) -0.09449(19) 0.0363(8) Uani 1 1 d .
H2A H 0.4020 0.4508 -0.1535 0.044 Uiso 1 1 calc R
H2B H 0.4864 0.5054 -0.0807 0.044 Uiso 1 1 calc R
C3 C 0.2988(4) 0.5612(3) -0.0810(2) 0.0395(8) Uani 1 1 d .
H3A H 0.3360 0.6291 -0.0616 0.047 Uiso 1 1 calc R
H3B H 0.2513 0.5740 -0.1338 0.047 Uiso 1 1 calc R
C4 C 0.2146(3) 0.5147(3) -0.0143(2) 0.0330(7) Uani 1 1 d .
C5 C 0.3959(3) 0.3627(2) 0.23290(17) 0.0229(6) Uani 1 1 d .
C6 C 0.4855(3) 0.3978(2) 0.30040(18) 0.0259(6) Uani 1 1 d .
H6A H 0.4457 0.3939 0.3569 0.031 Uiso 1 1 calc R
H6B H 0.5151 0.4712 0.2903 0.031 Uiso 1 1 calc R
C7 C 0.5939(3) 0.3181(2) 0.29257(19) 0.0270(6) Uani 1 1 d .
H7A H 0.6718 0.3534 0.2726 0.032 Uiso 1 1 calc R
H7B H 0.6111 0.2833 0.3474 0.032 Uiso 1 1 calc R
C8 C 0.5468(3) 0.2383(2) 0.22822(18) 0.0249(6) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.01990(16) 0.02076(16) 0.02083(16) 0.00173(7) 0.00091(7) 0.00037(7)
S1 0.0301(4) 0.0335(4) 0.0274(4) -0.0041(3) 0.0035(3) -0.0007(3)
S2 0.0251(3) 0.0253(3) 0.0281(4) -0.0019(3) 0.0015(3) 0.0025(3)
O1 0.0459(14) 0.0380(13) 0.0493(15) 0.0068(11) 0.0078(12) 0.0084(11)
O2 0.0306(11) 0.0310(11) 0.0447(13) -0.0071(10) -0.0045(10) 0.0059(9)
N1 0.0263(12) 0.0298(12) 0.0225(11) 0.0032(10) -0.0002(10) -0.0029(10)
N2 0.0206(11) 0.0228(11) 0.0206(11) 0.0007(9) 0.0002(9) -0.0020(9)
C1 0.0273(15) 0.0401(17) 0.0186(13) -0.0032(12) -0.0010(12) -0.0062(13)
C2 0.0359(18) 0.050(2) 0.0227(15) 0.0041(13) 0.0004(12) -0.0117(16)
C3 0.0404(18) 0.0401(18) 0.0380(18) 0.0072(15) -0.0040(15) -0.0067(15)
C4 0.0350(16) 0.0332(16) 0.0307(16) 0.0006(13) -0.0049(14) -0.0025(14)
C5 0.0240(13) 0.0234(13) 0.0214(13) 0.0029(10) 0.0061(11) -0.0022(11)
C6 0.0300(14) 0.0256(14) 0.0220(13) -0.0011(11) 0.0015(11) 0.0002(11)
C7 0.0263(14) 0.0286(14) 0.0261(15) -0.0001(11) 0.0006(12) -0.0021(11)
C8 0.0233(13) 0.0262(14) 0.0251(14) 0.0020(11) 0.0018(11) -0.0019(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
Mo1 Mo1 S1 96.23(2) 2 2
Mo1 Mo1 S2 97.739(19) 2 .
Mo1 Mo1 N1 96.08(7) 2 .
Mo1 Mo1 N2 94.62(6) 2 2
S1 Mo1 S2 165.98(3) 2 .
N1 Mo1 S1 89.96(7) . 2
N1 Mo1 S2 87.32(7) . .
N1 Mo1 N2 169.06(9) . 2
N2 Mo1 S1 91.13(6) 2 2
N2 Mo1 S2 89.00(6) 2 .
C1 S1 Mo1 101.55(11) . 2
C5 S2 Mo1 101.12(10) . .
C1 N1 Mo1 123.7(2) . .
C1 N1 C4 110.2(3) . .
C4 N1 Mo1 125.8(2) . .
C5 N2 Mo1 125.20(19) . 2
C5 N2 C8 109.1(2) . .
C8 N2 Mo1 125.61(18) . 2
N1 C1 S1 122.3(2) . .
N1 C1 C2 112.8(3) . .
C2 C1 S1 124.9(2) . .
C1 C2 H2A 111.1 . .
C1 C2 H2B 111.1 . .
C1 C2 C3 103.2(3) . .
H2A C2 H2B 109.1 . .
C3 C2 H2A 111.1 . .
C3 C2 H2B 111.1 . .
C2 C3 H3A 110.8 . .
C2 C3 H3B 110.8 . .
H3A C3 H3B 108.9 . .
C4 C3 C2 104.5(3) . .
C4 C3 H3A 110.8 . .
C4 C3 H3B 110.8 . .
O1 C4 N1 122.3(3) . .
O1 C4 C3 128.7(3) . .
N1 C4 C3 109.0(3) . .
N2 C5 S2 121.3(2) . .
N2 C5 C6 113.8(2) . .
C6 C5 S2 124.9(2) . .
C5 C6 H6A 111.2 . .
C5 C6 H6B 111.2 . .
C5 C6 C7 103.0(2) . .
H6A C6 H6B 109.1 . .
C7 C6 H6A 111.2 . .
C7 C6 H6B 111.2 . .
C6 C7 H7A 111.0 . .
C6 C7 H7B 111.0 . .
H7A C7 H7B 109.0 . .
C8 C7 C6 104.0(2) . .
C8 C7 H7A 111.0 . .
C8 C7 H7B 111.0 . .
O2 C8 N2 121.9(3) . .
O2 C8 C7 128.5(3) . .
N2 C8 C7 109.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 Mo1 2.1112(4) 2
Mo1 S1 2.4753(8) 2
Mo1 S2 2.4754(7) .
Mo1 N1 2.139(2) .
Mo1 N2 2.151(2) 2
S1 Mo1 2.4753(8) 2
S1 C1 1.676(3) .
S2 C5 1.686(3) .
O1 C4 1.209(4) .
O2 C8 1.195(4) .
N1 C1 1.323(4) .
N1 C4 1.430(4) .
N2 Mo1 2.151(2) 2
N2 C5 1.332(4) .
N2 C8 1.418(3) .
C1 C2 1.505(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C2 C3 1.539(5) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C3 C4 1.502(5) .
C5 C6 1.497(4) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C6 C7 1.531(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C7 C8 1.515(4) .
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
Mo1 Mo1 S2 C5 -1.07(9) 2
Mo1 Mo1 N1 C1 4.0(2) 2
Mo1 Mo1 N1 C4 -168.8(2) 2
Mo1 S1 C1 N1 -1.9(3) 2
Mo1 S1 C1 C2 176.2(2) 2
Mo1 S2 C5 N2 2.5(2) .
Mo1 S2 C5 C6 -177.3(2) .
Mo1 N1 C1 S1 -1.3(4) .
Mo1 N1 C1 C2 -179.53(19) .
Mo1 N1 C4 O1 -0.2(4) .
Mo1 N1 C4 C3 179.5(2) .
Mo1 N2 C5 S2 -3.2(3) 2
Mo1 N2 C5 C6 176.61(17) 2
Mo1 N2 C8 O2 -1.7(4) 2
Mo1 N2 C8 C7 178.85(17) 2
S1 Mo1 S2 C5 -175.90(13) 2
S1 Mo1 N1 C1 -92.2(2) 2
S1 Mo1 N1 C4 94.9(2) 2
S1 C1 C2 C3 -175.0(2) .
S2 Mo1 N1 C1 101.6(2) .
S2 Mo1 N1 C4 -71.3(2) .
S2 C5 C6 C7 -176.1(2) .
N1 Mo1 S2 C5 -96.85(12) .
N1 C1 C2 C3 3.2(3) .
N2 Mo1 S2 C5 93.46(11) 2
N2 Mo1 N1 C1 172.0(4) 2
N2 Mo1 N1 C4 -0.9(6) 2
N2 C5 C6 C7 4.1(3) .
C1 N1 C4 O1 -173.8(3) .
C1 N1 C4 C3 5.8(3) .
C1 C2 C3 C4 0.4(3) .
C2 C3 C4 O1 176.0(3) .
C2 C3 C4 N1 -3.6(3) .
C4 N1 C1 S1 172.6(2) .
C4 N1 C1 C2 -5.7(3) .
C5 N2 C8 O2 174.5(3) .
C5 N2 C8 C7 -5.0(3) .
C5 C6 C7 C8 -6.5(3) .
C6 C7 C8 O2 -172.2(3) .
C6 C7 C8 N2 7.3(3) .
C8 N2 C5 S2 -179.38(19) .
C8 N2 C5 C6 0.4(3) .
