#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:33:52 +0100 (vie 25 de mar de 2016) $
#$Revision: 180085 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/31/7053131.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_7053131
loop_
_publ_author_name
'Judmaier, Martina E.'
'Sala, Chris H.'
'Belaj, Ferdinand'
'Volpe, Manuel'
'Mösch-Zanetti, Nadia C.'
_publ_section_title
;
 Dimeric μ-oxo bridged molybdenum(vi) dioxo complexes as catalysts in the
 epoxidation of internal and terminal alkenes
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2139
_journal_paper_doi               10.1039/c3nj00115f
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C26 H42 Mo2 N4 O7, 2 (C H2 Cl2)'
_chemical_formula_sum            'C28 H46 Cl4 Mo2 N4 O7'
_chemical_formula_weight         884.37
_chemical_name_systematic
;
?
;
_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                98.171(2)
_cell_angle_beta                 90.647(2)
_cell_angle_gamma                92.937(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4666(6)
_cell_length_b                   14.8332(11)
_cell_length_c                   16.7476(12)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.95
_cell_measurement_theta_min      2.64
_cell_volume                     1833.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60456
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         34.35
_diffrn_reflns_theta_min         2.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.364
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         12236
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0276P)²+2.7382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                11100
_reflns_number_total             12236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00115f.txt
_cod_data_source_block           dimemo
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7053131
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 0.904237(18) 0.762943(9) 0.820215(8) 0.01129(4) Uani 1 1 d . . .
Mo2 Mo 0.717197(18) 0.799224(10) 0.622745(8) 0.01287(4) Uani 1 1 d . . .
O3 O 1.10723(17) 0.75689(10) 0.77266(8) 0.0175(2) Uani 1 1 d . . .
O2 O 0.91197(19) 0.86032(9) 0.88954(8) 0.0183(2) Uani 1 1 d . . .
O11 O 0.96007(17) 0.67802(9) 0.89503(7) 0.0146(2) Uani 1 1 d . . .
O4 O 0.71324(19) 0.68206(9) 0.59890(8) 0.0206(3) Uani 1 1 d . . .
O5 O 0.50069(18) 0.83149(11) 0.62822(9) 0.0229(3) Uani 1 1 d . . .
O41 O 0.75648(18) 0.82497(10) 0.51265(8) 0.0177(2) Uani 1 1 d . . .
O1 O 0.77318(16) 0.80340(9) 0.73454(7) 0.0138(2) Uani 1 1 d . . .
N21 N 0.8041(2) 0.62170(10) 0.75079(9) 0.0148(3) Uani 1 1 d . . .
H21 H 0.7620 0.6325 0.7007 0.018 Uiso 1 1 calc R . .
N22 N 0.6031(2) 0.73507(11) 0.86528(9) 0.0157(3) Uani 1 1 d . . .
N51 N 1.02808(19) 0.81283(10) 0.61760(9) 0.0132(2) Uani 1 1 d . . .
H51 H 1.0706 0.7972 0.6659 0.016 Uiso 1 1 calc R . .
N52 N 0.7995(2) 0.96023(11) 0.65745(9) 0.0159(3) Uani 1 1 d . . .
C1 C 1.0509(2) 0.60079(12) 0.88341(10) 0.0132(3) Uani 1 1 d . . .
C2 C 1.1468(2) 0.57955(12) 0.95080(10) 0.0144(3) Uani 1 1 d . . .
C3 C 1.2497(2) 0.50362(13) 0.94143(11) 0.0165(3) Uani 1 1 d . . .
H3 H 1.3166 0.4902 0.9865 0.020 Uiso 1 1 calc R . .
C4 C 1.2582(2) 0.44618(13) 0.86778(11) 0.0169(3) Uani 1 1 d . . .
C5 C 1.1568(2) 0.46671(12) 0.80346(11) 0.0160(3) Uani 1 1 d . . .
H5 H 1.1582 0.4275 0.7534 0.019 Uiso 1 1 calc R . .
C6 C 1.0527(2) 0.54306(12) 0.80969(10) 0.0142(3) Uani 1 1 d . . .
C7 C 0.9512(3) 0.55931(12) 0.73474(10) 0.0171(3) Uani 1 1 d . . .
H7A H 1.0366 0.5847 0.6979 0.020 Uiso 1 1 calc R . .
H7B H 0.9009 0.5000 0.7067 0.020 Uiso 1 1 calc R . .
C8 C 0.6492(2) 0.58247(13) 0.79098(11) 0.0184(3) Uani 1 1 d . . .
H8A H 0.6897 0.5604 0.8409 0.022 Uiso 1 1 calc R . .
H8B H 0.5914 0.5302 0.7548 0.022 Uiso 1 1 calc R . .
C9 C 0.5170(2) 0.65625(13) 0.81104(11) 0.0187(3) Uani 1 1 d . . .
H9A H 0.4747 0.6768 0.7607 0.022 Uiso 1 1 calc R . .
H9B H 0.4117 0.6313 0.8378 0.022 Uiso 1 1 calc R . .
C10 C 0.6045(3) 0.71583(14) 0.94964(11) 0.0212(4) Uani 1 1 d . . .
H10A H 0.6674 0.7666 0.9844 0.032 Uiso 1 1 calc R . .
H10B H 0.6660 0.6596 0.9527 0.032 Uiso 1 1 calc R . .
H10C H 0.4808 0.7085 0.9677 0.032 Uiso 1 1 calc R . .
C11 C 0.4968(3) 0.81623(14) 0.86229(12) 0.0208(3) Uani 1 1 d . . .
H11A H 0.3749 0.8039 0.8806 0.031 Uiso 1 1 calc R . .
H11B H 0.4917 0.8299 0.8068 0.031 Uiso 1 1 calc R . .
H11C H 0.5535 0.8685 0.8975 0.031 Uiso 1 1 calc R . .
C12 C 1.1367(2) 0.63975(14) 1.03034(10) 0.0185(3) Uani 1 1 d . . .
H12A H 1.2034 0.6137 1.0715 0.028 Uiso 1 1 calc R . .
H12B H 1.0110 0.6442 1.0459 0.028 Uiso 1 1 calc R . .
H12C H 1.1890 0.7007 1.0256 0.028 Uiso 1 1 calc R . .
C13 C 1.3676(3) 0.36289(15) 0.85904(13) 0.0246(4) Uani 1 1 d . . .
H13A H 1.3006 0.3132 0.8802 0.037 Uiso 1 1 calc R . .
H13B H 1.4810 0.3771 0.8893 0.037 Uiso 1 1 calc R . .
H13C H 1.3923 0.3442 0.8019 0.037 Uiso 1 1 calc R . .
C14 C 0.8707(2) 0.79464(12) 0.45417(10) 0.0161(3) Uani 1 1 d . . .
C15 C 0.8187(3) 0.80364(13) 0.37443(11) 0.0202(4) Uani 1 1 d . . .
C16 C 0.9303(3) 0.77275(14) 0.31165(11) 0.0252(4) Uani 1 1 d . . .
H16 H 0.8947 0.7779 0.2579 0.030 Uiso 1 1 calc R . .
C17 C 1.0924(3) 0.73457(14) 0.32492(12) 0.0254(4) Uani 1 1 d . . .
C18 C 1.1421(3) 0.72829(14) 0.40409(12) 0.0216(4) Uani 1 1 d . . .
H18 H 1.2533 0.7032 0.4142 0.026 Uiso 1 1 calc R . .
C19 C 1.0342(2) 0.75768(12) 0.46942(11) 0.0166(3) Uani 1 1 d . . .
C20 C 1.1011(2) 0.74703(13) 0.55286(11) 0.0169(3) Uani 1 1 d . . .
H20A H 1.0682 0.6843 0.5634 0.020 Uiso 1 1 calc R . .
H20B H 1.2336 0.7549 0.5546 0.020 Uiso 1 1 calc R . .
C21 C 1.0958(2) 0.90779(12) 0.61553(11) 0.0164(3) Uani 1 1 d . . .
H21A H 1.0775 0.9243 0.5609 0.020 Uiso 1 1 calc R . .
H21B H 1.2258 0.9142 0.6288 0.020 Uiso 1 1 calc R . .
C22 C 0.9948(2) 0.96986(12) 0.67653(11) 0.0174(3) Uani 1 1 d . . .
H22A H 1.0168 0.9542 0.7312 0.021 Uiso 1 1 calc R . .
H22B H 1.0385 1.0339 0.6761 0.021 Uiso 1 1 calc R . .
C23 C 0.7567(3) 1.01200(14) 0.59089(12) 0.0221(4) Uani 1 1 d . . .
H23A H 0.7843 1.0772 0.6083 0.033 Uiso 1 1 calc R . .
H23B H 0.6290 1.0019 0.5765 0.033 Uiso 1 1 calc R . .
H23C H 0.8285 0.9912 0.5439 0.033 Uiso 1 1 calc R . .
C24 C 0.7001(3) 0.99915(14) 0.72939(12) 0.0227(4) Uani 1 1 d . . .
H24A H 0.7340 1.0643 0.7428 0.034 Uiso 1 1 calc R . .
H24B H 0.7299 0.9677 0.7751 0.034 Uiso 1 1 calc R . .
H24C H 0.5709 0.9911 0.7178 0.034 Uiso 1 1 calc R . .
C25 C 0.6457(3) 0.84664(15) 0.35984(12) 0.0265(4) Uani 1 1 d . . .
H25A H 0.6260 0.8451 0.3017 0.040 Uiso 1 1 calc R . .
H25B H 0.6520 0.9101 0.3864 0.040 Uiso 1 1 calc R . .
H25C H 0.5464 0.8128 0.3819 0.040 Uiso 1 1 calc R . .
C26 C 1.2129(4) 0.70357(18) 0.25568(14) 0.0361(6) Uani 1 1 d . . .
H26A H 1.2594 0.7566 0.2321 0.054 Uiso 1 1 calc R . .
H26B H 1.1443 0.6617 0.2145 0.054 Uiso 1 1 calc R . .
H26C H 1.3132 0.6722 0.2755 0.054 Uiso 1 1 calc R . .
C1S C 0.8336(4) 0.95504(18) 0.07248(15) 0.0409(6) Uani 1 1 d D . .
H1S1 H 0.8166 0.9438 0.0131 0.049 Uiso 1 1 calc R . .
H1S2 H 0.8803 1.0189 0.0877 0.049 Uiso 1 1 calc R . .
Cl1 Cl 0.99009(16) 0.88130(7) 0.10145(5) 0.0673(3) Uani 1 1 d D . .
Cl2 Cl 0.62604(18) 0.93947(7) 0.11854(8) 0.0925(5) Uani 1 1 d D . .
C2S C 0.300(2) 0.4450(9) 0.5781(10) 0.132(9) Uani 0.45 1 d PD A 1
H2S1 H 0.2923 0.4224 0.5195 0.158 Uiso 0.45 1 calc PR A 1
H2S2 H 0.1812 0.4322 0.6013 0.158 Uiso 0.45 1 calc PR A 1
Cl3 Cl 0.3499(3) 0.56232(14) 0.59271(16) 0.0392(4) Uani 0.45 1 d PD A 1
Cl4 Cl 0.46295(19) 0.38730(9) 0.62352(9) 0.0372(3) Uani 0.45 1 d PD A 1
C3S C 0.2662(9) 0.4445(4) 0.5615(6) 0.0389(15) Uani 0.55 1 d PD B 2
H3S1 H 0.2292 0.4084 0.6045 0.047 Uiso 0.55 1 calc PR B 2
H3S2 H 0.3300 0.4047 0.5199 0.047 Uiso 0.55 1 calc PR B 2
Cl5 Cl 0.0624(2) 0.48903(9) 0.51512(10) 0.0534(3) Uani 0.55 1 d PD . 2
Cl6 Cl 0.4014(3) 0.53415(16) 0.60041(13) 0.0567(5) Uani 0.55 1 d PD B 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'
Cl Cl 0.1484 0.1585 '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
O2 Mo1 O3 108.13(7) .
O2 Mo1 O1 100.10(6) .
O3 Mo1 O1 96.64(6) .
O2 Mo1 O11 97.24(6) .
O3 Mo1 O11 95.08(6) .
O1 Mo1 O11 154.87(5) .
O2 Mo1 N21 160.08(6) .
O3 Mo1 N21 91.42(6) .
O1 Mo1 N21 80.85(5) .
O11 Mo1 N21 76.70(5) .
O2 Mo1 N22 86.42(6) .
O3 Mo1 N22 165.45(6) .
O1 Mo1 N22 80.76(5) .
O11 Mo1 N22 82.33(5) .
N21 Mo1 N22 74.04(5) .
O5 Mo2 O4 108.20(7) .
O5 Mo2 O1 100.15(6) .
O4 Mo2 O1 96.32(6) .
O5 Mo2 O41 96.00(6) .
O4 Mo2 O41 95.82(6) .
O1 Mo2 O41 155.63(6) .
O5 Mo2 N51 158.91(6) .
O4 Mo2 N51 92.54(6) .
O1 Mo2 N51 80.79(5) .
O41 Mo2 N51 77.63(5) .
O5 Mo2 N52 85.50(6) .
O4 Mo2 N52 166.28(6) .
O1 Mo2 N52 80.22(5) .
O41 Mo2 N52 83.00(5) .
N51 Mo2 N52 73.84(5) .
C1 O11 Mo1 130.31(11) .
C14 O41 Mo2 133.85(12) .
Mo2 O1 Mo1 151.12(8) .
C7 N21 C8 113.79(14) .
C7 N21 Mo1 112.08(11) .
C8 N21 Mo1 111.26(11) .
C10 N22 C11 107.65(15) .
C10 N22 C9 110.09(14) .
C11 N22 C9 109.08(15) .
C10 N22 Mo1 110.96(11) .
C11 N22 Mo1 110.36(11) .
C9 N22 Mo1 108.67(11) .
C21 N51 C20 113.06(14) .
C21 N51 Mo2 112.41(10) .
C20 N51 Mo2 112.56(11) .
C23 N52 C24 107.72(15) .
C23 N52 C22 110.23(14) .
C24 N52 C22 109.08(15) .
C23 N52 Mo2 111.74(12) .
C24 N52 Mo2 110.10(11) .
C22 N52 Mo2 107.95(11) .
O11 C1 C6 123.54(15) .
O11 C1 C2 116.37(15) .
C6 C1 C2 120.09(16) .
C3 C2 C1 118.92(16) .
C3 C2 C12 121.63(16) .
C1 C2 C12 119.45(16) .
C2 C3 C4 122.14(16) .
C5 C4 C3 117.63(17) .
C5 C4 C13 120.85(17) .
C3 C4 C13 121.49(17) .
C4 C5 C6 122.31(17) .
C5 C6 C1 118.82(16) .
C5 C6 C7 117.36(16) .
C1 C6 C7 123.80(16) .
N21 C7 C6 114.06(14) .
N21 C8 C9 108.21(14) .
N22 C9 C8 110.34(15) .
O41 C14 C19 123.45(16) .
O41 C14 C15 116.26(17) .
C19 C14 C15 120.28(17) .
C16 C15 C14 118.79(19) .
C16 C15 C25 121.87(18) .
C14 C15 C25 119.34(18) .
C15 C16 C17 122.15(18) .
C18 C17 C16 117.88(19) .
C18 C17 C26 121.1(2) .
C16 C17 C26 121.0(2) .
C17 C18 C19 122.3(2) .
C18 C19 C14 118.59(17) .
C18 C19 C20 117.77(17) .
C14 C19 C20 123.64(16) .
N51 C20 C19 113.51(15) .
N51 C21 C22 108.39(14) .
N52 C22 C21 110.41(15) .
Cl1 C1S Cl2 111.39(15) .
Cl3 C2S Cl4 111.2(9) .
Cl6 C3S Cl5 108.2(4) .
Cl5 Cl5 C3S 176.1(3) 2_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O2 1.7178(13) .
Mo1 O3 1.7206(13) .
Mo1 O1 1.9104(12) .
Mo1 O11 1.9548(12) .
Mo1 N21 2.3298(15) .
Mo1 N22 2.4138(15) .
Mo2 O5 1.7091(14) .
Mo2 O4 1.7256(14) .
Mo2 O1 1.9055(12) .
Mo2 O41 1.9577(13) .
Mo2 N51 2.3233(14) .
Mo2 N52 2.4221(16) .
O11 C1 1.353(2) .
O41 C14 1.350(2) .
N21 C7 1.475(2) .
N21 C8 1.480(2) .
N22 C10 1.481(2) .
N22 C11 1.482(2) .
N22 C9 1.488(2) .
N51 C21 1.477(2) .
N51 C20 1.481(2) .
N52 C23 1.481(2) .
N52 C24 1.484(2) .
N52 C22 1.484(2) .
C1 C6 1.400(2) .
C1 C2 1.411(2) .
C2 C3 1.387(3) .
C2 C12 1.500(2) .
C3 C4 1.400(3) .
C4 C5 1.387(2) .
C4 C13 1.507(3) .
C5 C6 1.399(2) .
C6 C7 1.514(2) .
C8 C9 1.516(3) .
C14 C19 1.399(3) .
C14 C15 1.413(2) .
C15 C16 1.390(3) .
C15 C25 1.502(3) .
C16 C17 1.391(3) .
C17 C18 1.390(3) .
C17 C26 1.510(3) .
C18 C19 1.399(3) .
C19 C20 1.511(3) .
C21 C22 1.511(3) .
C1S Cl1 1.751(3) .
C1S Cl2 1.758(3) .
C2S Cl3 1.744(13) .
C2S Cl4 1.752(15) .
C3S Cl6 1.676(7) .
C3S Cl5 1.891(9) .
Cl5 Cl5 1.140(3) 2_566
