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#$Date: 2025-08-21 00:40:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301839 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/12/4331276.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_4331276
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            'C9 H14 Mo N6 O5'
_chemical_formula_weight         382.20
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.085(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.4830(8)
_cell_length_b                   9.9708(4)
_cell_length_c                   14.7921(7)
_cell_measurement_temperature    100(2)
_cell_volume                     2619.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13061
_diffrn_reflns_theta_full        28.90
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    1.036
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_F_000             1536
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0317
_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)+(0.0413P)²+7.8413P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                2591
_reflns_number_total             3143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301282q_si_001.cif
_cod_data_source_block           shelxl
_cod_database_code               4331276
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mo Mo 0.656468(14) 0.22547(3) 0.222577(17) 0.01115(9) Uani 1 1 d .
O4 O 0.60802(12) 0.0789(2) 0.18927(16) 0.0169(5) Uani 1 1 d .
O6 O 0.93168(13) 0.7231(2) 0.61144(17) 0.0182(5) Uani 1 1 d .
O3 O 0.64533(12) 0.3252(2) 0.12601(15) 0.0170(5) Uani 1 1 d .
O2 O 0.76034(11) 0.1527(2) 0.24408(15) 0.0148(5) Uani 1 1 d .
N4 N 0.84311(13) 0.3379(2) 0.45395(17) 0.0111(5) Uani 1 1 d .
N2 N 0.81965(14) 0.2058(3) 0.31606(19) 0.0142(5) Uani 1 1 d .
O1 O 0.58800(11) 0.3121(2) 0.28730(15) 0.0156(5) Uani 1 1 d .
N5 N 0.73136(13) 0.4434(2) 0.47993(18) 0.0119(5) Uani 1 1 d .
N6 N 0.84968(13) 0.4792(3) 0.58004(18) 0.0118(5) Uani 1 1 d .
N3 N 0.61780(13) 0.3951(3) 0.36534(18) 0.0147(5) Uani 1 1 d .
N1 N 0.72260(13) 0.3071(2) 0.34602(17) 0.0112(5) Uani 1 1 d .
C9 C 0.85066(17) 0.7230(3) 0.5855(2) 0.0159(6) Uani 1 1 d .
H7A H 0.8313 0.7284 0.5176 0.019 Uiso 1 1 calc R
H7B H 0.8330 0.8010 0.6123 0.019 Uiso 1 1 calc R
C5 C 0.56360(17) 0.4441(3) 0.4111(2) 0.0174(7) Uani 1 1 d .
H4A H 0.5141 0.4406 0.3679 0.026 Uiso 1 1 calc R
H4B H 0.5755 0.5351 0.4309 0.026 Uiso 1 1 calc R
H4C H 0.5650 0.3893 0.4649 0.026 Uiso 1 1 calc R
C2 C 0.79807(16) 0.2850(3) 0.3764(2) 0.0103(6) Uani 1 1 d .
C7 C 0.95869(17) 0.6096(3) 0.5706(2) 0.0144(6) Uani 1 1 d .
H9A H 1.0133 0.6112 0.5880 0.017 Uiso 1 1 calc R
H9B H 0.9406 0.6150 0.5026 0.017 Uiso 1 1 calc R
C6 C 0.93234(16) 0.4796(3) 0.6035(2) 0.0121(6) Uani 1 1 d .
H8A H 0.9494 0.4044 0.5732 0.014 Uiso 1 1 calc R
H8B H 0.9535 0.4704 0.6710 0.014 Uiso 1 1 calc R
C3 C 0.80729(16) 0.4196(3) 0.5018(2) 0.0109(6) Uani 1 1 d .
C8 C 0.82118(17) 0.5966(3) 0.6203(2) 0.0127(6) Uani 1 1 d .
H6A H 0.8381 0.5930 0.6884 0.015 Uiso 1 1 calc R
H6B H 0.7666 0.5968 0.6010 0.015 Uiso 1 1 calc R
C4 C 0.89220(17) 0.1457(3) 0.3270(2) 0.0160(6) Uani 1 1 d .
H5A H 0.8913 0.0937 0.2721 0.024 Uiso 1 1 calc R
H5B H 0.9041 0.0885 0.3813 0.024 Uiso 1 1 calc R
H5C H 0.9296 0.2148 0.3350 0.024 Uiso 1 1 calc R
C1 C 0.69205(16) 0.3844(3) 0.4017(2) 0.0118(6) Uani 1 1 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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O3 Mo O4 108.92(11)
O3 Mo O1 101.84(10)
O4 Mo O1 99.07(10)
O3 Mo O2 103.49(10)
O4 Mo O2 97.99(10)
O1 Mo O2 142.77(9)
O3 Mo N1 114.57(10)
O4 Mo N1 136.51(10)
O1 Mo N1 72.65(9)
O2 Mo N1 72.18(9)
C7 O6 C9 110.1(2)
N2 O2 Mo 119.94(16)
C2 N4 C3 114.0(2)
C2 N2 O2 114.6(2)
C2 N2 C4 127.9(3)
O2 N2 C4 115.9(2)
N3 O1 Mo 119.76(16)
C1 N5 C3 114.1(3)
C3 N6 C6 121.7(2)
C3 N6 C8 120.7(2)
C6 N6 C8 111.5(2)
C1 N3 O1 114.3(2)
C1 N3 C5 127.6(3)
O1 N3 C5 114.9(2)
C2 N1 C1 116.8(2)
C2 N1 Mo 122.1(2)
C1 N1 Mo 121.08(19)
O6 C9 C8 110.8(2)
N4 C2 N2 125.6(3)
N4 C2 N1 124.3(3)
N2 C2 N1 110.1(3)
O6 C7 C6 111.1(2)
N6 C6 C7 109.4(2)
N6 C3 N4 117.4(3)
N6 C3 N5 116.2(3)
N4 C3 N5 126.3(3)
N6 C8 C9 108.7(2)
N5 C1 N3 125.0(3)
N5 C1 N1 124.2(3)
N3 C1 N1 110.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo O3 1.705(2)
Mo O4 1.713(2)
Mo O1 1.984(2)
Mo O2 1.994(2)
Mo N1 2.063(2)
O6 C7 1.436(4)
O6 C9 1.439(4)
O2 N2 1.403(3)
N4 C2 1.325(4)
N4 C3 1.365(4)
N2 C2 1.333(4)
N2 C4 1.436(4)
O1 N3 1.403(3)
N5 C1 1.321(4)
N5 C3 1.371(4)
N6 C3 1.343(4)
N6 C6 1.470(4)
N6 C8 1.475(4)
N3 C1 1.332(4)
N3 C5 1.441(4)
N1 C2 1.360(4)
N1 C1 1.360(4)
C9 C8 1.518(4)
C7 C6 1.512(4)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139138137
