#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/06/7010602.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_7010602
loop_
_publ_author_name
'Schollhammer, Philippe'
'Le Hénanf, Marc'
'Le Roy-Le Floch, Christine'
'Pétillon, François Y.'
'Talarmin, Jean'
'Muir, Kenneth W.'
_publ_section_title
;
 Acetonitrile hydration versus molybdenum oxidation at the sulfur-rich
 bimetallic site {MoIII2Cp2(μ-SMe)3}+. Crystal structure of the
 μ-η1 ∶ η1-amidato complex
 [Mo2Cp2(μ-MeCONH)(μ-SMe)3]
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1573
_journal_paper_doi               10.1039/b100986i
_journal_year                    2001
_chemical_formula_moiety         'C15 H23 Mo2 N O S3'
_chemical_formula_sum            'C15 H23 Mo2 N O S3'
_chemical_formula_weight         521.4
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             2000-09-21T15:48:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.790(6)
_cell_length_b                   13.841(5)
_cell_length_c                   16.717(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      10.1
_cell_volume                     3653(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP (Farrugia, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            5371
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 129
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.716
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.7657
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.97
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0794P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                1793
_reflns_number_total             3767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100986i.txt
_cod_data_source_block           km1299
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               7010602
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Mo1 Mo 0.59140(5) 0.19895(6) -0.13183(5) 0.0296(2) Uani 1 d . . .
Mo2 Mo 0.68610(5) 0.31260(6) -0.22977(5) 0.0293(2) Uani 1 d . . .
S1 S 0.74322(17) 0.17444(19) -0.15555(15) 0.0368(6) Uani 1 d . . .
S2 S 0.61104(17) 0.16899(17) -0.27382(16) 0.0358(6) Uani 1 d . . .
S3 S 0.53786(17) 0.34416(18) -0.19567(17) 0.0362(6) Uani 1 d . . .
O1 O 0.6314(4) 0.2967(5) -0.0387(4) 0.0379(16) Uani 1 d . . .
N1 N 0.7081(6) 0.3922(6) -0.1198(5) 0.035(2) Uani 1 d . . .
H1 H 0.753(7) 0.415(8) -0.101(7) 0.05(3) Uiso 1 d . . .
C1 C 0.8102(7) 0.2060(9) -0.0706(6) 0.048(3) Uani 1 d . . .
H1A H 0.8283 0.272 -0.0756 0.072 Uiso 1 calc R . .
H1B H 0.8588 0.1644 -0.0696 0.072 Uiso 1 calc R . .
H1C H 0.7786 0.1984 -0.0219 0.072 Uiso 1 calc R . .
C2 C 0.5183(7) 0.1958(9) -0.3339(7) 0.048(3) Uani 1 d . . .
H2A H 0.4988 0.26 -0.322 0.072 Uiso 1 calc R . .
H2B H 0.4743 0.1502 -0.3218 0.072 Uiso 1 calc R . .
H2C H 0.5326 0.1915 -0.3895 0.072 Uiso 1 calc R . .
C3 C 0.5142(8) 0.4425(8) -0.1296(7) 0.057(3) Uani 1 d . . .
H3A H 0.5225 0.4222 -0.0753 0.085 Uiso 1 calc R . .
H3B H 0.4564 0.4621 -0.137 0.085 Uiso 1 calc R . .
H3C H 0.5511 0.4958 -0.1412 0.085 Uiso 1 calc R . .
C4 C 0.6779(7) 0.3702(8) -0.0502(7) 0.038(3) Uani 1 d . . .
C5 C 0.6995(7) 0.4314(7) 0.0241(6) 0.054(3) Uani 1 d . . .
H5A H 0.7374 0.396 0.0581 0.081 Uiso 1 calc R . .
H5B H 0.6484 0.4458 0.0529 0.081 Uiso 1 calc R . .
H5C H 0.726 0.4906 0.0077 0.081 Uiso 1 calc R . .
C11 C 0.4735(7) 0.1096(8) -0.1391(6) 0.053(3) Uani 1 d R . .
H11 H 0.4395 0.1152 -0.1843 0.063 Uiso 1 calc R . .
C12 C 0.4658(7) 0.1630(8) -0.0700(7) 0.049(3) Uani 1 d . . .
H12 H 0.4265 0.2117 -0.0608 0.059 Uiso 1 calc R . .
C13 C 0.5258(8) 0.1319(10) -0.0178(8) 0.059(4) Uani 1 d . . .
H13 H 0.5328 0.1546 0.0342 0.071 Uiso 1 calc R . .
C14 C 0.5728(9) 0.0642(9) -0.0521(10) 0.071(4) Uani 1 d . . .
H14 H 0.6193 0.034 -0.0288 0.086 Uiso 1 calc R . .
C15 C 0.5414(9) 0.0452(8) -0.1296(8) 0.059(4) Uani 1 d . . .
H15 H 0.5614 0 -0.1662 0.071 Uiso 1 calc R . .
C21 C 0.7504(15) 0.4442(9) -0.2837(8) 0.091(6) Uani 1 d . . .
H21 H 0.7534 0.5021 -0.2556 0.109 Uiso 1 calc R . .
C22 C 0.6845(10) 0.4168(11) -0.3414(8) 0.071(4) Uani 1 d . . .
H22 H 0.6367 0.4513 -0.3569 0.085 Uiso 1 calc R . .
C23 C 0.7108(8) 0.3289(9) -0.3661(7) 0.050(3) Uani 1 d . . .
H23 H 0.6825 0.2931 -0.4049 0.06 Uiso 1 calc R . .
C24 C 0.7803(10) 0.2984(13) -0.3304(8) 0.074(4) Uani 1 d . . .
H24 H 0.8062 0.239 -0.3394 0.089 Uiso 1 calc R . .
C25 C 0.8083(9) 0.3669(16) -0.2784(10) 0.085(5) Uani 1 d . . .
H25 H 0.856 0.3634 -0.2459 0.102 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 0 '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 0.006 '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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 7 -3
-3 3 -7
5 -5 -3
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0660
0 0 -1 0.0660
1 1 1 0.0550
-1 -1 -1 0.0550
-1 1 0 0.0860
1 -1 0 0.0860
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 C11 129.0(3) . . ?
O1 Mo1 C15 132.7(4) . . ?
C11 Mo1 C15 36.3(4) . . ?
O1 Mo1 C12 93.7(4) . . ?
C11 Mo1 C12 35.4(4) . . ?
C15 Mo1 C12 59.2(4) . . ?
O1 Mo1 C14 97.3(5) . . ?
C11 Mo1 C14 58.6(5) . . ?
C15 Mo1 C14 35.9(5) . . ?
C12 Mo1 C14 56.9(5) . . ?
O1 Mo1 C13 78.0(4) . . ?
C11 Mo1 C13 57.4(4) . . ?
C15 Mo1 C13 57.7(5) . . ?
C12 Mo1 C13 33.9(4) . . ?
C14 Mo1 C13 33.0(5) . . ?
O1 Mo1 S3 84.3(2) . . ?
C11 Mo1 S3 98.3(3) . . ?
C15 Mo1 S3 131.5(4) . . ?
C12 Mo1 S3 94.4(3) . . ?
C14 Mo1 S3 151.3(4) . . ?
C13 Mo1 S3 121.9(4) . . ?
O1 Mo1 S2 140.77(19) . . ?
C11 Mo1 S2 87.6(2) . . ?
C15 Mo1 S2 84.3(3) . . ?
C12 Mo1 S2 120.9(3) . . ?
C14 Mo1 S2 116.2(4) . . ?
C13 Mo1 S2 141.1(3) . . ?
S3 Mo1 S2 75.89(9) . . ?
O1 Mo1 S1 85.24(19) . . ?
C11 Mo1 S1 136.7(3) . . ?
C15 Mo1 S1 102.3(4) . . ?
C12 Mo1 S1 152.7(3) . . ?
C14 Mo1 S1 96.1(4) . . ?
C13 Mo1 S1 120.3(4) . . ?
S3 Mo1 S1 112.56(10) . . ?
S2 Mo1 S1 72.17(9) . . ?
O1 Mo1 Mo2 84.86(18) . . ?
C11 Mo1 Mo2 138.1(3) . . ?
C15 Mo1 Mo2 138.0(3) . . ?
C12 Mo1 Mo2 150.9(3) . . ?
C14 Mo1 Mo2 152.1(4) . . ?
C13 Mo1 Mo2 162.8(3) . . ?
S3 Mo1 Mo2 56.48(7) . . ?
S2 Mo1 Mo2 55.95(7) . . ?
S1 Mo1 Mo2 56.31(7) . . ?
N1 Mo2 C25 89.9(6) . . ?
N1 Mo2 C24 124.8(5) . . ?
C25 Mo2 C24 35.4(6) . . ?
N1 Mo2 C21 81.8(4) . . ?
C25 Mo2 C21 36.5(6) . . ?
C24 Mo2 C21 58.6(6) . . ?
N1 Mo2 C23 139.0(4) . . ?
C25 Mo2 C23 57.5(5) . . ?
C24 Mo2 C23 33.4(4) . . ?
C21 Mo2 C23 57.2(4) . . ?
N1 Mo2 C22 111.2(5) . . ?
C25 Mo2 C22 60.9(6) . . ?
C24 Mo2 C22 58.0(6) . . ?
C21 Mo2 C22 36.9(6) . . ?
C23 Mo2 C22 33.5(4) . . ?
N1 Mo2 S2 138.6(2) . . ?
C25 Mo2 S2 126.1(6) . . ?
C24 Mo2 S2 91.4(5) . . ?
C21 Mo2 S2 138.9(4) . . ?
C23 Mo2 S2 82.2(3) . . ?
C22 Mo2 S2 104.8(4) . . ?
N1 Mo2 S3 82.3(3) . . ?
C25 Mo2 S3 148.7(6) . . ?
C24 Mo2 S3 145.1(4) . . ?
C21 Mo2 S3 112.1(6) . . ?
C23 Mo2 S3 111.8(3) . . ?
C22 Mo2 S3 93.7(4) . . ?
S2 Mo2 S3 75.53(9) . . ?
N1 Mo2 S1 84.7(2) . . ?
C25 Mo2 S1 97.4(5) . . ?
C24 Mo2 S1 93.8(4) . . ?
C21 Mo2 S1 131.4(6) . . ?
C23 Mo2 S1 120.7(3) . . ?
C22 Mo2 S1 151.8(4) . . ?
S2 Mo2 S1 72.22(10) . . ?
S3 Mo2 S1 111.91(9) . . ?
N1 Mo2 Mo1 82.6(2) . . ?
C25 Mo2 Mo1 153.2(5) . . ?
C24 Mo2 Mo1 139.6(5) . . ?
C21 Mo2 Mo1 161.6(4) . . ?
C23 Mo2 Mo1 137.7(3) . . ?
C22 Mo2 Mo1 145.5(4) . . ?
S2 Mo2 Mo1 55.99(8) . . ?
S3 Mo2 Mo1 55.75(7) . . ?
S1 Mo2 Mo1 56.37(7) . . ?
C1 S1 Mo2 114.9(4) . . ?
C1 S1 Mo1 114.0(4) . . ?
Mo2 S1 Mo1 67.32(7) . . ?
C2 S2 Mo2 113.2(4) . . ?
C2 S2 Mo1 113.7(4) . . ?
Mo2 S2 Mo1 68.06(7) . . ?
C3 S3 Mo1 115.5(4) . . ?
C3 S3 Mo2 118.6(4) . . ?
Mo1 S3 Mo2 67.77(7) . . ?
C4 O1 Mo1 124.3(7) . . ?
C4 N1 Mo2 125.7(7) . . ?
O1 C4 N1 122.6(9) . . ?
O1 C4 C5 116.5(9) . . ?
N1 C4 C5 120.9(9) . . ?
C12 C11 C15 108.3(11) . . ?
C12 C11 Mo1 74.4(6) . . ?
C15 C11 Mo1 73.1(6) . . ?
C13 C12 C11 107.9(11) . . ?
C13 C12 Mo1 75.8(7) . . ?
C11 C12 Mo1 70.2(6) . . ?
C14 C13 C12 109.6(13) . . ?
C14 C13 Mo1 71.5(7) . . ?
C12 C13 Mo1 70.3(7) . . ?
C13 C14 C15 109.4(13) . . ?
C13 C14 Mo1 75.6(7) . . ?
C15 C14 Mo1 70.5(6) . . ?
C11 C15 C14 104.7(11) . . ?
C11 C15 Mo1 70.7(5) . . ?
C14 C15 Mo1 73.6(6) . . ?
C25 C21 C22 107.8(12) . . ?
C25 C21 Mo2 69.9(7) . . ?
C22 C21 Mo2 74.8(7) . . ?
C23 C22 C21 102.4(13) . . ?
C23 C22 Mo2 71.8(7) . . ?
C21 C22 Mo2 68.3(7) . . ?
C24 C23 C22 114.0(14) . . ?
C24 C23 Mo2 70.4(7) . . ?
C22 C23 Mo2 74.7(7) . . ?
C23 C24 C25 109.6(15) . . ?
C23 C24 Mo2 76.2(8) . . ?
C25 C24 Mo2 71.1(7) . . ?
C24 C25 C21 106.1(14) . . ?
C24 C25 Mo2 73.5(8) . . ?
C21 C25 Mo2 73.5(8) . . ?
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 2.157(7) . ?
Mo1 C11 2.238(8) . ?
Mo1 C15 2.270(10) . ?
Mo1 C12 2.291(11) . ?
Mo1 C14 2.310(11) . ?
Mo1 C13 2.360(12) . ?
Mo1 S3 2.428(3) . ?
Mo1 S2 2.430(3) . ?
Mo1 S1 2.453(3) . ?
Mo1 Mo2 2.7186(14) . ?
Mo2 N1 2.171(9) . ?
Mo2 C25 2.224(12) . ?
Mo2 C24 2.254(12) . ?
Mo2 C21 2.271(11) . ?
Mo2 C23 2.323(12) . ?
Mo2 C22 2.359(12) . ?
Mo2 S2 2.428(3) . ?
Mo2 S3 2.448(3) . ?
Mo2 S1 2.452(3) . ?
S1 C1 1.823(11) . ?
S2 C2 1.814(10) . ?
S3 C3 1.792(10) . ?
O1 C4 1.269(12) . ?
N1 C4 1.293(14) . ?
C4 C5 1.543(13) . ?
C11 C12 1.376(14) . ?
C11 C15 1.403(17) . ?
C12 C13 1.359(17) . ?
C13 C14 1.326(18) . ?
C14 C15 1.412(18) . ?
C21 C25 1.41(2) . ?
C21 C22 1.47(2) . ?
C22 C23 1.351(18) . ?
C23 C24 1.319(17) . ?
C24 C25 1.36(2) . ?
