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#$Date: 2016-03-23 20:37:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179415 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/12/4331278.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_4331278
loop_
_publ_author_name
'Marios Stylianou'
'Vladimiros A. Nikolakis'
'George I. Chilas'
'Tamas Jakusch'
'Tiverios Vaimakis'
'Tamas Kiss'
'Michael P. Sigalas'
'Anastasios D. Keramidas'
'Themistoklis A. Kabanos'
_publ_section_title
;
 Molybdenum(VI) Coordination Chemistry of the N,N-Disubstituted
 Bis(hydroxylamido)-1,3,5-triazine Ligand, H2bihyat. Water-Assisted
 Activation of the MoVI=O Bond and Reversible Dimerization of
 cis-[MoVIO2(bihyat)] to [MoVI2O4(bihyat)2(H2O)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13138
_journal_page_last               13147
_journal_paper_doi               10.1021/ic301282q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C11 H14 D7 Mo N7 O7'
_chemical_formula_weight         466.33
_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                99.284(5)
_cell_angle_beta                 103.021(5)
_cell_angle_gamma                101.044(6)
_cell_formula_units_Z            2
_cell_length_a                   7.7201(5)
_cell_length_b                   9.0995(7)
_cell_length_c                   13.0492(8)
_cell_measurement_temperature    100(2)
_cell_volume                     856.31(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.487
_diffrn_measured_fraction_theta_max 0.487
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2871
_diffrn_reflns_theta_full        28.83
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.818
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_F_000             468
_refine_diff_density_max         1.082
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         2192
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0929P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                1936
_reflns_number_total             2192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301282q_si_003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        856.30(10)
_cod_database_code               4331278
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
Mo Mo 0.48425(7) 0.48750(6) 0.37873(3) 0.0115(2) Uani 1 1 d .
O3 O 0.4076(7) 0.6438(5) 0.3530(3) 0.0176(10) Uani 1 1 d .
O5 O 0.5909(7) 0.2679(5) 0.3963(3) 0.0136(9) Uani 1 1 d D
O6 O 0.5263(7) -0.0044(6) -0.2276(4) 0.0207(11) Uani 1 1 d .
O2 O 0.2399(6) 0.3314(5) 0.2960(3) 0.0140(9) Uani 1 1 d .
O1W O 0.9588(7) 0.2968(6) 0.4364(4) 0.0240(11) Uani 1 1 d D
O1 O 0.7488(7) 0.5625(5) 0.3631(3) 0.0130(9) Uani 1 1 d .
N6 N 0.5012(8) 0.2577(6) -0.0860(4) 0.0152(11) Uani 1 1 d .
N3 N 0.7880(9) 0.5245(7) 0.2643(4) 0.0165(13) Uani 1 1 d .
N4 N 0.3349(8) 0.2666(6) 0.0397(4) 0.0139(12) Uani 1 1 d .
N2 N 0.2005(8) 0.2864(7) 0.1834(4) 0.0169(12) Uani 1 1 d .
O4 O 0.6515(6) 0.5715(5) 0.5203(3) 0.0130(9) Uani 1 1 d .
N5 N 0.6604(8) 0.3883(6) 0.0858(4) 0.0134(11) Uani 1 1 d .
N7 N 0.0614(10) 0.9694(7) 0.3268(5) 0.0285(14) Uani 1 1 d .
N1 N 0.4905(8) 0.4109(6) 0.2189(4) 0.0152(11) Uani 1 1 d .
C4 C 0.0225(10) 0.1867(8) 0.1308(5) 0.0168(13) Uani 1 1 d D
C5 C 0.9742(11) 0.5781(9) 0.2616(6) 0.0206(16) Uani 1 1 d D
C9 C 0.6840(11) 0.0868(9) -0.1472(5) 0.0215(15) Uani 1 1 d .
C11 C 0.1586(10) 1.0126(7) 0.4102(5) 0.0189(13) Uani 1 1 d D
C3 C 0.4996(10) 0.3070(7) 0.0181(5) 0.0137(13) Uani 1 1 d .
C7 C 0.3622(10) -0.0018(9) -0.1931(5) 0.0206(15) Uani 1 1 d .
C8 C 0.6718(10) 0.2531(8) -0.1170(5) 0.0153(13) Uani 1 1 d .
C2 C 0.3400(9) 0.3206(8) 0.1424(5) 0.0139(12) Uani 1 1 d .
C10 C 0.2799(12) 1.0684(9) 0.5173(5) 0.0269(16) Uani 1 1 d D
C1 C 0.6471(9) 0.4394(7) 0.1858(4) 0.0113(12) Uani 1 1 d .
C6 C 0.3393(10) 0.1606(9) -0.1684(5) 0.0170(13) Uani 1 1 d .
H7A H 0.373(12) -0.028(9) -0.111(5) 0.020 Uiso 1 1 d .
H7B H 0.301(12) -0.036(9) -0.244(6) 0.020 Uiso 1 1 d .
H6A H 0.311(11) 0.209(8) -0.254(5) 0.020 Uiso 1 1 d .
H6B H 0.233(11) 0.166(10) -0.145(5) 0.020 Uiso 1 1 d .
H9A H 0.782(10) 0.068(8) -0.169(5) 0.002(16) Uiso 1 1 d .
H9B H 0.694(12) 0.035(8) -0.080(5) 0.016(18) Uiso 1 1 d .
H8A H 0.803(12) 0.320(9) -0.054(5) 0.022(19) Uiso 1 1 d .
H8B H 0.688(11) 0.300(8) -0.175(5) 0.009(16) Uiso 1 1 d .
H5A H 1.023(12) 0.681(3) 0.289(5) 0.03(2) Uiso 1 1 d D
H4A H 0.013(13) 0.160(9) 0.058(2) 0.03(2) Uiso 1 1 d D
H4B H -0.048(14) 0.258(10) 0.133(8) 0.08(4) Uiso 1 1 d D
H5B H 1.036(10) 0.537(9) 0.315(4) 0.03(2) Uiso 1 1 d D
H5C H 0.987(11) 0.573(9) 0.193(3) 0.03(2) Uiso 1 1 d D
H4C H -0.002(15) 0.105(7) 0.164(7) 0.07(3) Uiso 1 1 d D
H10B D 0.230(5) 1.129(5) 0.555(2) 0.03(2) Uiso 1 1 d D
H10C D 0.289(7) 0.987(3) 0.546(3) 0.07(4) Uiso 1 1 d D
H10A D 0.386(3) 1.116(6) 0.513(2) 0.05(3) Uiso 1 1 d D
H5G D 0.525(10) 0.186(7) 0.339(4) 0.04(3) Uiso 1 1 d D
H2Q D 1.036(10) 0.357(9) 0.502(3) 0.05(3) Uiso 1 1 d D
H1W D 1.025(11) 0.316(13) 0.385(5) 0.10(4) Uiso 1 1 d D
H5F D 0.712(5) 0.288(13) 0.391(8) 0.11(5) Uiso 1 1 d D
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 '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
O3 Mo O4 100.45(19) . 2_666
O3 Mo O4 100.6(2) . .
O4 Mo O4 74.4(2) 2_666 .
O3 Mo O2 95.0(2) . .
O4 Mo O2 70.35(16) 2_666 .
O4 Mo O2 143.50(16) . .
O3 Mo O1 97.1(2) . .
O4 Mo O1 143.18(17) 2_666 .
O4 Mo O1 70.66(16) . .
O2 Mo O1 139.85(15) . .
O3 Mo N1 93.9(2) . .
O4 Mo N1 139.4(2) 2_666 .
O4 Mo N1 139.6(2) . .
O2 Mo N1 70.77(19) . .
O1 Mo N1 70.3(2) . .
O3 Mo O5 174.29(16) . .
O4 Mo O5 84.28(16) 2_666 .
O4 Mo O5 83.73(17) . .
O2 Mo O5 83.56(17) . .
O1 Mo O5 80.70(17) . .
N1 Mo O5 80.37(18) . .
O3 Mo Mo 103.24(13) . 2_666
O4 Mo Mo 37.22(13) 2_666 2_666
O4 Mo Mo 37.21(12) . 2_666
O2 Mo Mo 107.07(10) . 2_666
O1 Mo Mo 107.13(11) . 2_666
N1 Mo Mo 162.83(16) . 2_666
O5 Mo Mo 82.47(10) . 2_666
C9 O6 C7 111.3(5) . .
N2 O2 Mo 118.8(3) . .
N3 O1 Mo 120.5(4) . .
C3 N6 C8 122.1(6) . .
C3 N6 C6 122.7(6) . .
C8 N6 C6 112.4(5) . .
C1 N3 O1 114.6(6) . .
C1 N3 C5 128.8(5) . .
O1 N3 C5 116.6(5) . .
C2 N4 C3 112.9(6) . .
C2 N2 O2 115.4(5) . .
C2 N2 C4 128.1(5) . .
O2 N2 C4 115.5(5) . .
Mo O4 Mo 105.6(2) 2_666 .
C3 N5 C1 112.9(6) . .
C1 N1 C2 115.2(5) . .
C1 N1 Mo 122.6(5) . .
C2 N1 Mo 122.1(4) . .
H4A C4 H4B 102(8) . .
H4A C4 H4C 115(8) . .
H4B C4 H4C 118(9) . .
H4A C4 N2 109(6) . .
H4B C4 N2 99(7) . .
H4C C4 N2 112(7) . .
H5C C5 H5A 99(6) . .
H5C C5 H5B 127(7) . .
H5A C5 H5B 101(7) . .
H5C C5 N3 113(5) . .
H5A C5 N3 115(6) . .
H5B C5 N3 101(5) . .
H9A C9 H9B 102(6) . .
H9A C9 O6 106(4) . .
H9B C9 O6 106(4) . .
H9A C9 C8 118(5) . .
H9B C9 C8 111(4) . .
O6 C9 C8 112.2(6) . .
N7 C11 C10 179.0(7) . .
N5 C3 N4 128.6(5) . .
N5 C3 N6 116.1(6) . .
N4 C3 N6 115.3(6) . .
H7B C7 H7A 133(8) . .
H7B C7 O6 96(7) . .
H7A C7 O6 113(4) . .
H7B C7 C6 105(7) . .
H7A C7 C6 99(4) . .
O6 C7 C6 110.5(6) . .
H8B C8 H8A 99(6) . .
H8B C8 N6 116(5) . .
H8A C8 N6 116(4) . .
H8B C8 C9 107(4) . .
H8A C8 C9 109(4) . .
N6 C8 C9 109.6(6) . .
N2 C2 N4 123.4(7) . .
N2 C2 N1 111.3(5) . .
N4 C2 N1 125.2(6) . .
N3 C1 N5 122.9(6) . .
N3 C1 N1 112.1(5) . .
N5 C1 N1 125.1(6) . .
H6B C6 H6A 103(6) . .
H6B C6 N6 110(5) . .
H6A C6 N6 112(4) . .
H6B C6 C7 112(5) . .
H6A C6 C7 109(3) . .
N6 C6 C7 109.9(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo O3 1.695(4) .
Mo O4 1.938(4) 2_666
Mo O4 1.938(4) .
Mo O2 2.075(5) .
Mo O1 2.093(5) .
Mo N1 2.104(5) .
Mo O5 2.327(4) .
Mo Mo 3.0866(8) 2_666
O6 C9 1.424(9) .
O6 C7 1.440(8) .
O2 N2 1.406(6) .
O1 N3 1.394(6) .
N6 C3 1.365(7) .
N6 C8 1.468(7) .
N6 C6 1.470(9) .
N3 C1 1.323(8) .
N3 C5 1.437(9) .
N4 C2 1.340(7) .
N4 C3 1.358(9) .
N2 C2 1.314(9) .
N2 C4 1.442(9) .
O4 Mo 1.938(4) 2_666
N5 C3 1.346(9) .
N5 C1 1.347(7) .
N7 C11 1.134(9) .
N1 C1 1.366(8) .
N1 C2 1.367(9) .
C4 H4A 0.92(2) .
C4 H4B 0.92(2) .
C4 H4C 0.93(2) .
C5 H5C 0.91(2) .
C5 H5A 0.92(2) .
C5 H5B 0.92(2) .
C9 H9A 0.90(7) .
C9 H9B 1.05(6) .
C9 C8 1.527(9) .
C11 C10 1.445(10) .
C7 H7B 0.70(7) .
C7 H7A 1.12(6) .
C7 C6 1.514(10) .
C8 H8B 0.94(6) .
C8 H8A 1.14(8) .
C6 H6B 0.94(8) .
C6 H6A 1.26(7) .
