#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:50:11 +0100 (vie 25 de mar de 2016) $
#$Revision: 180098 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/44/7054468.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_7054468
loop_
_publ_author_name
'Vrdoljak, Višnja'
'Pisk, Jana'
'Agustin, Dominique'
'Novak, Predrag'
'Parlov Vuković, Jelena'
'Matković-Čalogović, Dubravka'
_publ_section_title
;
 Dioxomolybdenum(vi) and dioxotungsten(vi) complexes chelated with the ONO
 tridentate hydrazone ligand: synthesis, structure and catalytic
 epoxidation activity
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              6176
_journal_paper_doi               10.1039/C4NJ01394H
_journal_volume                  38
_journal_year                    2014
_chemical_formula_sum            'C17 H15 Mo N3 O6'
_chemical_formula_weight         453.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.342(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.97920(10)
_cell_length_b                   10.3039(3)
_cell_length_c                   21.3511(9)
_cell_measurement_reflns_used    3057
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6570
_cell_measurement_theta_min      4.4050
_cell_volume                     871.62(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6290
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.926
_diffrn_reflns_theta_min         4.315
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.315
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0450P)²+0.1248P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                3308
_reflns_number_total             3373
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4nj01394h2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7054467--7054471.cif.'
_cod_database_code               7054468
#BEGIN Tags that were not found in dictionaries:
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.852(2) 0.2951(6) 0.7221(3) 0.0284(16) Uani 1 1 d . .
C2 C 0.8727(19) 0.1726(7) 0.6920(3) 0.0245(15) Uani 1 1 d . .
C3 C 0.916(2) 0.1652(7) 0.6276(3) 0.0347(19) Uani 1 1 d . .
C4 C 0.942(3) 0.2787(9) 0.5941(4) 0.059(3) Uani 1 1 d . .
H4 H 0.9764 0.2745 0.5507 0.071 Uiso 1 1 calc R U
C5 C 0.920(4) 0.3997(9) 0.6229(4) 0.076(4) Uani 1 1 d . .
H5 H 0.9395 0.4769 0.5992 0.091 Uiso 1 1 calc R U
C6 C 0.870(3) 0.4068(8) 0.6861(4) 0.053(3) Uani 1 1 d . .
H6 H 0.8488 0.4893 0.7052 0.064 Uiso 1 1 calc R U
C7 C 0.8045(18) 0.3050(6) 0.7876(3) 0.0223(14) Uani 1 1 d . .
H7 H 0.7418 0.3869 0.8034 0.027 Uiso 1 1 calc R U
C8 C 0.8227(14) 0.1302(6) 0.9225(3) 0.0143(12) Uani 1 1 d . .
C9 C 0.7578(15) 0.1302(6) 0.9882(3) 0.0147(12) Uani 1 1 d . .
C10 C 0.8337(14) 0.0210(7) 1.0266(3) 0.0145(15) Uani 1 1 d . .
H10 H 0.9432 -0.0517 1.0102 0.017 Uiso 1 1 calc R U
C11 C 0.7512(15) 0.0187(8) 1.0874(3) 0.0163(15) Uani 1 1 d . .
H11 H 0.8005 -0.0559 1.1128 0.020 Uiso 1 1 calc R U
C12 C 0.5959(17) 0.1252(6) 1.1119(3) 0.0179(12) Uani 1 1 d . .
C13 C 0.5275(15) 0.2350(6) 1.0759(3) 0.0170(13) Uani 1 1 d . .
H13 H 0.4256 0.3084 1.0934 0.020 Uiso 1 1 calc R U
C14 C 0.6083(17) 0.2376(6) 1.0145(3) 0.0181(13) Uani 1 1 d . .
H14 H 0.5617 0.3132 0.9898 0.022 Uiso 1 1 calc R U
C15 C 1.006(2) 0.0324(9) 0.5402(3) 0.048(3) Uani 1 1 d . .
H15A H 1.0066 -0.0595 0.5284 0.071 Uiso 1 1 calc R U
H15B H 0.8361 0.0787 0.5124 0.071 Uiso 1 1 calc R U
H15C H 1.2291 0.0699 0.5360 0.071 Uiso 1 1 calc R U
C16 C 0.476(3) 0.7493(8) 0.6118(4) 0.041(2) Uani 1 1 d . .
C17 C 0.339(3) 0.7866(11) 0.6698(4) 0.053(3) Uani 1 1 d . .
H17A H 0.1834 0.8596 0.6617 0.079 Uiso 1 1 calc R U
H17B H 0.5238 0.8124 0.7009 0.079 Uiso 1 1 calc R U
H17C H 0.2181 0.7129 0.6861 0.079 Uiso 1 1 calc R U
N1 N 0.8424(15) 0.2091(5) 0.8265(3) 0.0160(11) Uani 1 1 d . .
N2 N 0.7796(14) 0.2355(5) 0.8880(2) 0.0179(11) Uani 1 1 d . .
N3 N 0.587(2) 0.7187(9) 0.5675(4) 0.060(2) Uani 1 1 d . .
O1 O 0.3873(9) 0.0149(8) 0.80870(18) 0.0220(11) Uani 1 1 d . .
O3 O 0.8431(12) 0.0602(4) 0.72273(19) 0.0172(9) Uani 1 1 d . .
O4 O 0.9121(11) 0.0185(6) 0.89684(17) 0.0151(10) Uani 1 1 d . .
O7 O 0.9270(16) 0.0444(5) 0.6038(2) 0.0375(15) Uani 1 1 d . .
O6 O 0.5100(13) 0.1155(4) 1.1731(2) 0.0231(10) Uani 1 1 d . .
H6A H 0.4145 0.1842 1.1829 0.035 Uiso 1 1 calc R U
O2 O 0.8749(11) -0.1614(4) 0.7995(2) 0.0185(10) Uani 1 1 d . .
Mo Mo 0.95627(10) 0.00136(5) 0.80672(2) 0.01208(11) 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C6 C1 C2 118.4(6) . .
C6 C1 C7 120.0(6) . .
C2 C1 C7 121.6(6) . .
O3 C2 C3 117.2(6) . .
O3 C2 C1 122.2(6) . .
C3 C2 C1 120.6(6) . .
O7 C3 C4 125.6(7) . .
O7 C3 C2 115.5(6) . .
C4 C3 C2 118.9(7) . .
C3 C4 C5 121.2(8) . .
C6 C5 C4 119.8(8) . .
C5 C6 C1 121.0(7) . .
N1 C7 C1 123.7(6) . .
N2 C8 O4 120.5(6) . .
N2 C8 C9 121.1(6) . .
O4 C8 C9 118.3(5) . .
C14 C9 C10 118.3(6) . .
C14 C9 C8 120.6(6) . .
C10 C9 C8 121.1(5) . .
C11 C10 C9 120.6(7) . .
C10 C11 C12 120.0(7) . .
C13 C12 O6 122.1(6) . .
C13 C12 C11 120.7(6) . .
O6 C12 C11 117.2(5) . .
C14 C13 C12 119.6(6) . .
C13 C14 C9 120.8(6) . .
N3 C16 C17 178.5(11) . .
C7 N1 N2 116.0(6) . .
C7 N1 Mo 128.7(5) . .
N2 N1 Mo 115.1(4) . .
C8 N2 N1 110.1(5) . .
Mo O1 Mo 171.5(5) 1_455 .
C2 O3 Mo 135.3(4) . .
C8 O4 Mo 122.1(4) . .
C3 O7 C15 117.1(6) . .
O2 Mo O1 105.2(3) . 1_655
O2 Mo O3 101.58(19) . .
O1 Mo O3 98.3(2) 1_655 .
O2 Mo O4 98.2(2) . .
O1 Mo O4 98.60(18) 1_655 .
O3 Mo O4 149.48(19) . .
O2 Mo N1 156.14(19) . .
O1 Mo N1 97.9(3) 1_655 .
O3 Mo N1 80.74(18) . .
O4 Mo N1 71.9(2) . .
O2 Mo O1 83.2(3) . .
O1 Mo O1 171.5(5) 1_655 .
O3 Mo O1 81.34(18) . .
O4 Mo O1 78.19(16) . .
N1 Mo O1 73.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.389(10) .
C1 C2 1.423(9) .
C1 C7 1.432(9) .
C2 O3 1.342(8) .
C2 C3 1.403(9) .
C3 O7 1.347(9) .
C3 C4 1.380(11) .
C4 C5 1.396(12) .
C5 C6 1.384(11) .
C7 N1 1.290(8) .
C8 N2 1.314(8) .
C8 O4 1.337(8) .
C8 C9 1.451(9) .
C9 C14 1.398(9) .
C9 C10 1.408(9) .
C10 C11 1.368(8) .
C11 C12 1.386(10) .
C12 C13 1.381(8) .
C12 O6 1.383(7) .
C13 C14 1.379(9) .
C15 O7 1.429(8) .
C16 N3 1.126(11) .
C16 C17 1.450(12) .
N1 N2 1.386(7) .
N1 Mo 2.236(5) .
O1 Mo 1.717(4) 1_455
O1 Mo 2.273(3) .
O3 Mo 1.907(4) .
O4 Mo 1.956(4) .
O2 Mo 1.713(4) .
Mo O1 1.717(4) 1_655
