#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:41:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179984 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/78/7027878.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027878
loop_
_publ_author_name
'Brown, Emma J.'
'Whitwood, Adrian C.'
'Walton, Paul H.'
'Duhme-Klair, Anne-K.'
_publ_section_title
;
 Synthesis and characterisation of cis-dioxomolybdenum(vi) complexes of
 N-substituted 3-hydroxy-2-pyridinonesElectronic supplementary information
 (ESI) available: ORTEP plot and structural details of [MoO2(Lb)2]. See
 http://www.rsc.org/suppdata/dt/b4/b407221a/
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              2458
_journal_page_last               2462
_journal_paper_doi               10.1039/b407221a
_journal_year                    2004
_chemical_formula_moiety         'C16 H16 Mo2 N2 O14, 2(C6 H16 N)'
_chemical_formula_sum            'C28 H48 Mo2 N4 O14'
_chemical_formula_weight         856.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.5560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0526(5)
_cell_length_b                   14.6016(7)
_cell_length_c                   12.0634(5)
_cell_measurement_reflns_used    7385
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.46
_cell_volume                     1770.06(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11952
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0246
_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)+(0.0400P)²+0.5874P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                3689
_reflns_number_total             4082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b407221asup1.cif
_cod_data_source_block           cpd4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027878
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
H1 H 0.624(3) 0.4146(17) 0.196(2) 0.059(8) Uiso 1 1 d .
C14 C 0.8289(4) 0.3243(3) 0.1400(3) 0.1200(16) Uani 1 1 d .
H14A H 0.7844 0.3489 0.0752 0.180 Uiso 1 1 calc R
H14B H 0.8733 0.2684 0.1212 0.180 Uiso 1 1 calc R
H14C H 0.8932 0.3678 0.1679 0.180 Uiso 1 1 calc R
Mo1 Mo 0.617340(14) 0.574395(10) 0.006554(12) 0.03304(7) Uani 1 1 d .
O2 O 0.56354(14) 0.70500(9) -0.04892(11) 0.0417(3) Uani 1 1 d .
O1 O 0.47570(14) 0.63509(8) 0.13677(10) 0.0390(3) Uani 1 1 d .
N1 N 0.37513(16) 0.76886(10) 0.18566(12) 0.0367(3) Uani 1 1 d .
C2 C 0.49467(18) 0.75928(12) 0.01531(14) 0.0343(3) Uani 1 1 d .
O4 O 0.2303(2) 0.58622(13) 0.33732(17) 0.0770(6) Uani 1 1 d .
C1 C 0.44792(17) 0.71705(12) 0.11538(13) 0.0324(3) Uani 1 1 d .
C3 C 0.4660(2) 0.84961(13) -0.00453(16) 0.0433(4) Uani 1 1 d .
H3 H 0.4960 0.8780 -0.0682 0.052 Uiso 1 1 calc R
C6 C 0.3325(2) 0.72501(15) 0.28758(16) 0.0461(4) Uani 1 1 d .
H6A H 0.2906 0.7709 0.3332 0.055 Uiso 1 1 calc R
H6B H 0.4108 0.7030 0.3282 0.055 Uiso 1 1 calc R
C5 C 0.3464(2) 0.85971(13) 0.16423(17) 0.0432(4) Uani 1 1 d .
H5 H 0.2964 0.8933 0.2136 0.052 Uiso 1 1 calc R
C7 C 0.2380(2) 0.64688(15) 0.27138(18) 0.0496(5) Uani 1 1 d .
C4 C 0.3909(2) 0.89943(14) 0.07181(18) 0.0478(5) Uani 1 1 d .
H4 H 0.3719 0.9608 0.0580 0.057 Uiso 1 1 calc R
O6 O 0.57991(12) 0.46022(8) 0.06434(10) 0.0348(3) Uani 1 1 d .
O7 O 0.69461(17) 0.55596(11) -0.11564(13) 0.0540(4) Uani 1 1 d .
O3 O 0.16163(16) 0.65593(11) 0.18121(16) 0.0606(4) Uani 1 1 d .
C8 C 0.0635(3) 0.58384(19) 0.1587(3) 0.0790(9) Uani 1 1 d .
H8A H 0.1053 0.5250 0.1668 0.118 Uiso 1 1 calc R
H8B H 0.0281 0.5903 0.0844 0.118 Uiso 1 1 calc R
H8C H -0.0074 0.5889 0.2101 0.118 Uiso 1 1 calc R
O5 O 0.74200(16) 0.60935(13) 0.09656(15) 0.0613(4) Uani 1 1 d .
N2 N 0.65198(19) 0.38838(13) 0.25696(14) 0.0495(4) Uani 1 1 d .
C9 C 0.5282(3) 0.3595(2) 0.3121(2) 0.0703(7) Uani 1 1 d .
H9A H 0.4820 0.3152 0.2652 0.084 Uiso 1 1 calc R
H9B H 0.4706 0.4124 0.3190 0.084 Uiso 1 1 calc R
C11 C 0.7298(3) 0.4575(2) 0.3201(2) 0.0749(8) Uani 1 1 d .
H11A H 0.8027 0.4782 0.2754 0.090 Uiso 1 1 calc R
H11B H 0.7679 0.4290 0.3863 0.090 Uiso 1 1 calc R
C10 C 0.5521(4) 0.3177(2) 0.4264(2) 0.1006(13) Uani 1 1 d .
H10A H 0.6121 0.2668 0.4210 0.151 Uiso 1 1 calc R
H10B H 0.4691 0.2969 0.4548 0.151 Uiso 1 1 calc R
H10C H 0.5902 0.3629 0.4755 0.151 Uiso 1 1 calc R
C13 C 0.7314(4) 0.3058(2) 0.2251(3) 0.0900(10) Uani 1 1 d .
H13A H 0.7776 0.2822 0.2907 0.108 Uiso 1 1 calc R
H13B H 0.6707 0.2587 0.1981 0.108 Uiso 1 1 calc R
C12 C 0.6498(5) 0.5384(2) 0.3532(3) 0.0971(12) Uani 1 1 d .
H12A H 0.5990 0.5604 0.2902 0.146 Uiso 1 1 calc R
H12B H 0.7082 0.5859 0.3802 0.146 Uiso 1 1 calc R
H12C H 0.5905 0.5210 0.4106 0.146 Uiso 1 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 0.0000 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
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
O7 Mo1 O5 104.61(9) . .
O7 Mo1 O6 106.59(6) . .
O5 Mo1 O6 100.51(7) . .
O7 Mo1 O2 89.27(6) . .
O5 Mo1 O2 96.30(7) . .
O6 Mo1 O2 152.96(5) . .
O7 Mo1 O6 93.13(7) . 3_665
O5 Mo1 O6 162.18(7) . 3_665
O6 Mo1 O6 75.44(5) . 3_665
O2 Mo1 O6 82.08(5) . 3_665
O7 Mo1 O1 161.04(6) . .
O5 Mo1 O1 84.78(7) . .
O6 Mo1 O1 87.38(5) . .
O2 Mo1 O1 73.15(5) . .
O6 Mo1 O1 77.75(5) 3_665 .
O7 Mo1 Mo1 101.66(6) . 3_665
O5 Mo1 Mo1 139.22(6) . 3_665
O6 Mo1 Mo1 41.52(4) . 3_665
O2 Mo1 Mo1 114.78(4) . 3_665
O6 Mo1 Mo1 33.92(3) 3_665 3_665
O1 Mo1 Mo1 80.12(3) . 3_665
C2 O2 Mo1 119.77(11) . .
C1 O1 Mo1 111.21(11) . .
C1 N1 C5 121.97(16) . .
C1 N1 C6 117.06(16) . .
C5 N1 C6 120.93(16) . .
O2 C2 C3 126.00(17) . .
O2 C2 C1 114.98(15) . .
C3 C2 C1 119.01(16) . .
O1 C1 N1 121.43(16) . .
O1 C1 C2 120.22(15) . .
N1 C1 C2 118.34(15) . .
C2 C3 C4 119.80(18) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
N1 C6 C7 115.12(17) . .
N1 C6 H6A 108.5 . .
C7 C6 H6A 108.5 . .
N1 C6 H6B 108.5 . .
C7 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
C4 C5 N1 119.82(17) . .
C4 C5 H5 120.1 . .
N1 C5 H5 120.1 . .
O4 C7 O3 125.1(2) . .
O4 C7 C6 122.1(2) . .
O3 C7 C6 112.62(19) . .
C5 C4 C3 121.05(18) . .
C5 C4 H4 119.5 . .
C3 C4 H4 119.5 . .
Mo1 O6 Mo1 104.56(5) . 3_665
C7 O3 C8 117.1(2) . .
O3 C8 H8A 109.5 . .
O3 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
O3 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C11 N2 C9 113.6(2) . .
C11 N2 C13 113.8(2) . .
C9 N2 C13 110.1(2) . .
C11 N2 H1 107.0(17) . .
C9 N2 H1 104.4(19) . .
C13 N2 H1 107.3(18) . .
N2 C9 C10 113.9(3) . .
N2 C9 H9A 108.8 . .
C10 C9 H9A 108.8 . .
N2 C9 H9B 108.8 . .
C10 C9 H9B 108.8 . .
H9A C9 H9B 107.7 . .
N2 C11 C12 113.5(3) . .
N2 C11 H11A 108.9 . .
C12 C11 H11A 108.9 . .
N2 C11 H11B 108.9 . .
C12 C11 H11B 108.9 . .
H11A C11 H11B 107.7 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C14 C13 N2 113.7(3) . .
C14 C13 H13A 108.8 . .
N2 C13 H13A 108.8 . .
C14 C13 H13B 108.8 . .
N2 C13 H13B 108.8 . .
H13A C13 H13B 107.7 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C14 C13 1.464(5) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
Mo1 O7 1.7061(14) .
Mo1 O5 1.7135(16) .
Mo1 O6 1.8497(12) .
Mo1 O2 2.0874(13) .
Mo1 O6 2.1969(13) 3_665
Mo1 O1 2.3242(13) .
Mo1 Mo1 3.2079(3) 3_665
O2 C2 1.318(2) .
O1 C1 1.254(2) .
N1 C1 1.364(2) .
N1 C5 1.381(2) .
N1 C6 1.461(2) .
C2 C3 1.370(3) .
C2 C1 1.445(2) .
O4 C7 1.194(3) .
C3 C4 1.409(3) .
C3 H3 0.9300 .
C6 C7 1.494(3) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C5 C4 1.344(3) .
C5 H5 0.9300 .
C7 O3 1.321(3) .
C4 H4 0.9300 .
O6 Mo1 2.1969(13) 3_665
O3 C8 1.463(3) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
N2 C11 1.476(3) .
N2 C9 1.487(3) .
N2 C13 1.502(3) .
N2 H1 0.87(3) .
C9 C10 1.522(4) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C11 C12 1.490(5) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
N2 O6 2.633(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O7 Mo1 O2 C2 -179.89(15) . .
O5 Mo1 O2 C2 -75.28(15) . .
O6 Mo1 O2 C2 53.0(2) . .
O6 Mo1 O2 C2 86.84(14) 3_665 .
O1 Mo1 O2 C2 7.31(13) . .
Mo1 Mo1 O2 C2 77.60(14) 3_665 .
O7 Mo1 O1 C1 -28.8(3) . .
O5 Mo1 O1 C1 92.10(13) . .
O6 Mo1 O1 C1 -167.09(12) . .
O2 Mo1 O1 C1 -6.11(12) . .
O6 Mo1 O1 C1 -91.42(12) 3_665 .
Mo1 Mo1 O1 C1 -125.93(12) 3_665 .
Mo1 O2 C2 C3 171.94(16) . .
Mo1 O2 C2 C1 -7.5(2) . .
Mo1 O1 C1 N1 -174.52(13) . .
Mo1 O1 C1 C2 4.6(2) . .
C5 N1 C1 O1 178.54(17) . .
C6 N1 C1 O1 0.8(3) . .
C5 N1 C1 C2 -0.6(3) . .
C6 N1 C1 C2 -178.33(16) . .
O2 C2 C1 O1 1.3(2) . .
C3 C2 C1 O1 -178.23(18) . .
O2 C2 C1 N1 -179.58(16) . .
C3 C2 C1 N1 0.9(3) . .
O2 C2 C3 C4 179.98(19) . .
C1 C2 C3 C4 -0.6(3) . .
C1 N1 C6 C7 -64.4(2) . .
C5 N1 C6 C7 117.8(2) . .
C1 N1 C5 C4 -0.1(3) . .
C6 N1 C5 C4 177.6(2) . .
N1 C6 C7 O4 153.4(2) . .
N1 C6 C7 O3 -30.1(3) . .
N1 C5 C4 C3 0.5(3) . .
C2 C3 C4 C5 -0.1(3) . .
O7 Mo1 O6 Mo1 -88.94(8) . 3_665
O5 Mo1 O6 Mo1 162.22(7) . 3_665
O2 Mo1 O6 Mo1 34.71(14) . 3_665
O6 Mo1 O6 Mo1 0.0 3_665 3_665
O1 Mo1 O6 Mo1 78.02(5) . 3_665
O4 C7 O3 C8 -2.5(3) . .
C6 C7 O3 C8 -178.8(2) . .
C11 N2 C9 C10 -59.6(3) . .
C13 N2 C9 C10 69.4(3) . .
C9 N2 C11 C12 -51.9(3) . .
C13 N2 C11 C12 -179.0(3) . .
C11 N2 C13 C14 -70.3(3) . .
C9 N2 C13 C14 160.8(3) . .
