#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/20/7012052.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_7012052
loop_
_publ_author_name
'Dinda, Rupam'
'Sengupta, Parbati'
'Ghosh, Saktiprosad'
'Mayer-Figge, Heike'
'Sheldrick, William S.'
_publ_section_title
;
 A family of mononuclear molybdenum-(vi), and -(iv) oxo complexes with
 a tridentate (ONO) ligand
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4434
_journal_paper_doi               10.1039/b207129k
_journal_year                    2002
_chemical_formula_sum            'C16 H16 Mo N3 O5'
_chemical_formula_weight         426.26
_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                 109.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.019(2)
_cell_length_b                   9.804(2)
_cell_length_c                   15.004(3)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      7.5
_cell_volume                     1665.5(6)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        XDISK
_computing_molecular_graphics    'Siemens SHELXTL-PLUS (VMS)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Siemens P4 4-circle-diffractometer'
_diffrn_measurement_method       'Profile fitted'
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3072
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        20
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.50254
_exptl_absorpt_correction_T_min  0.46095
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            'pail yellow-orange'
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       ?0.0000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0320P)²+0.4940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                2312
_reflns_number_total             2926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207129k.txt
_cod_data_source_block           rd1
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1665.4(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C16 H16 N3 O5 Mo'
_cod_database_code               7012052
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.10340(3) 0.28532(3) 0.19880(2) 0.02966(11) Uani 1 1 d . . .
O1 O 0.0301(2) 0.4272(2) 0.21434(18) 0.0402(6) Uani 1 1 d . . .
O2 O 0.1999(2) 0.2458(3) 0.30694(19) 0.0527(8) Uani 1 1 d . . .
O3 O 0.2140(2) 0.3579(2) 0.14335(19) 0.0403(6) Uani 1 1 d . . .
O4 O -0.0205(2) 0.1476(2) 0.19514(16) 0.0323(5) Uani 1 1 d . . .
O5 O -0.0211(2) 0.3046(2) 0.04124(16) 0.0356(6) Uani 1 1 d . . .
N1 N 0.1404(2) 0.0957(3) 0.1307(2) 0.0299(6) Uani 1 1 d . . .
N2 N 0.0615(2) -0.0124(3) 0.1234(2) 0.0330(7) Uani 1 1 d . . .
C2 C 0.2278(3) 0.0705(4) 0.1018(3) 0.0357(8) Uani 1 1 d D . .
H2 H 0.238(3) -0.0168(17) 0.082(2) 0.043 Uiso 1 1 d D . .
C3 C -0.0189(3) 0.0252(3) 0.1591(2) 0.0289(7) Uani 1 1 d . . .
C11 C -0.1277(3) 0.3877(4) 0.0084(3) 0.0361(8) Uani 1 1 d D . .
H111 H -0.103(3) 0.4782(19) 0.033(3) 0.054(5) Uiso 1 1 d D . .
H112 H -0.153(3) 0.392(4) -0.0606(8) 0.054(5) Uiso 1 1 d D . .
C12 C -0.2227(3) 0.3294(4) 0.0406(3) 0.0506(11) Uani 1 1 d . . .
H121 H -0.1968 0.3289 0.1084 0.054(5) Uiso 1 1 calc R . .
H122 H -0.2396 0.2377 0.0174 0.054(5) Uiso 1 1 calc R . .
H123 H -0.2927 0.3840 0.0165 0.054(5) Uiso 1 1 calc R . .
C21 C 0.3163(3) 0.1699(4) 0.1018(3) 0.0359(8) Uani 1 1 d . . .
C22 C 0.4151(4) 0.1272(4) 0.0790(3) 0.0460(10) Uani 1 1 d D . .
H22 H 0.416(3) 0.0352(15) 0.064(3) 0.046(11) Uiso 1 1 d D . .
C23 C 0.5021(4) 0.2180(6) 0.0786(3) 0.0550(11) Uani 1 1 d . . .
H23 H 0.567(4) 0.186(4) 0.066(3) 0.071(15) Uiso 1 1 d . . .
C24 C 0.4920(4) 0.3529(5) 0.0996(3) 0.0505(10) Uani 1 1 d D . .
H24 H 0.550(3) 0.415(3) 0.100(3) 0.055(12) Uiso 1 1 d D . .
C25 C 0.3959(3) 0.3993(4) 0.1218(3) 0.0398(9) Uani 1 1 d D . .
H25 H 0.380(3) 0.4887(17) 0.134(3) 0.045(11) Uiso 1 1 d D . .
C26 C 0.3078(3) 0.3086(3) 0.1232(2) 0.0335(8) Uani 1 1 d . . .
C31 C -0.1138(3) -0.0694(3) 0.1593(2) 0.0292(7) Uani 1 1 d . . .
C32 C -0.2159(3) -0.0145(4) 0.1725(3) 0.0387(9) Uani 1 1 d D . .
H32 H -0.217(3) 0.0786(13) 0.183(3) 0.046 Uiso 1 1 d D . .
C33 C -0.3075(3) -0.0971(4) 0.1759(3) 0.0433(9) Uani 1 1 d D . .
H33 H -0.377(2) -0.058(4) 0.176(3) 0.053(12) Uiso 1 1 d D . .
C34 C -0.2993(4) -0.2360(4) 0.1662(3) 0.0471(10) Uani 1 1 d D . .
H34 H -0.357(3) -0.297(3) 0.170(3) 0.057 Uiso 1 1 d D . .
C35 C -0.1999(4) -0.2917(4) 0.1543(3) 0.0408(9) Uani 1 1 d D . .
H35 H -0.191(3) -0.3860(13) 0.151(3) 0.049 Uiso 1 1 d D . .
C36 C -0.1056(3) -0.2110(4) 0.1506(2) 0.0298(7) Uani 1 1 d . . .
N5 N -0.0074(3) -0.2749(3) 0.1389(2) 0.0359(7) Uani 1 1 d . . .
H51 H -0.0058 -0.3622 0.1341 0.043 Uiso 1 1 calc R . .
H52 H 0.0514 -0.2268 0.1365 0.043 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
_geom_angle_publ_flag
O2 Mo1 O1 105.97(13) . . ?
O2 Mo1 O3 98.52(13) . . ?
O1 Mo1 O3 102.79(11) . . ?
O2 Mo1 O4 97.85(12) . . ?
O1 Mo1 O4 98.09(11) . . ?
O3 Mo1 O4 148.68(10) . . ?
O2 Mo1 N1 94.04(12) . . ?
O1 Mo1 N1 158.78(11) . . ?
O3 Mo1 N1 80.67(10) . . ?
O4 Mo1 N1 71.69(9) . . ?
O2 Mo1 O5 170.38(11) . . ?
O1 Mo1 O5 83.54(10) . . ?
O3 Mo1 O5 80.45(10) . . ?
O4 Mo1 O5 78.98(9) . . ?
N1 Mo1 O5 76.35(9) . . ?
C26 O3 Mo1 135.5(2) . . ?
C3 O4 Mo1 120.9(2) . . ?
C11 O5 Mo1 125.3(2) . . ?
C2 N1 N2 115.8(3) . . ?
C2 N1 Mo1 128.5(2) . . ?
N2 N1 Mo1 115.60(19) . . ?
C3 N2 N1 109.1(3) . . ?
N1 C2 C21 123.7(3) . . ?
N1 C2 H2 120(2) . . ?
C21 C2 H2 116(2) . . ?
N2 C3 O4 122.7(3) . . ?
N2 C3 C31 120.2(3) . . ?
O4 C3 C31 117.1(3) . . ?
O5 C11 C12 110.9(3) . . ?
O5 C11 H111 105(2) . . ?
C12 C11 H111 113(2) . . ?
O5 C11 H112 108(2) . . ?
C12 C11 H112 111(2) . . ?
H111 C11 H112 108(3) . . ?
C11 C12 H121 109.5 . . ?
C11 C12 H122 109.5 . . ?
H121 C12 H122 109.5 . . ?
C11 C12 H123 109.5 . . ?
H121 C12 H123 109.5 . . ?
H122 C12 H123 109.5 . . ?
C22 C21 C26 118.4(3) . . ?
C22 C21 C2 118.8(3) . . ?
C26 C21 C2 122.8(3) . . ?
C23 C22 C21 121.0(4) . . ?
C23 C22 H22 124(2) . . ?
C21 C22 H22 115(2) . . ?
C24 C23 C22 119.7(4) . . ?
C24 C23 H23 121(3) . . ?
C22 C23 H23 119(3) . . ?
C23 C24 C25 121.2(4) . . ?
C23 C24 H24 121(3) . . ?
C25 C24 H24 118(3) . . ?
C24 C25 C26 119.7(4) . . ?
C24 C25 H25 127(2) . . ?
C26 C25 H25 113(2) . . ?
O3 C26 C25 118.2(3) . . ?
O3 C26 C21 121.8(3) . . ?
C25 C26 C21 120.0(3) . . ?
C36 C31 C32 118.8(3) . . ?
C36 C31 C3 123.1(3) . . ?
C32 C31 C3 118.1(3) . . ?
C33 C32 C31 121.5(4) . . ?
C33 C32 H32 121(2) . . ?
C31 C32 H32 118(2) . . ?
C34 C33 C32 119.4(4) . . ?
C34 C33 H33 121(3) . . ?
C32 C33 H33 119(3) . . ?
C33 C34 C35 120.0(4) . . ?
C33 C34 H34 123(3) . . ?
C35 C34 H34 117(3) . . ?
C34 C35 C36 122.1(4) . . ?
C34 C35 H35 121(2) . . ?
C36 C35 H35 117(2) . . ?
C35 C36 C31 118.3(3) . . ?
C35 C36 N5 118.8(3) . . ?
C31 C36 N5 123.0(3) . . ?
C36 N5 H51 120.0 . . ?
C36 N5 H52 120.0 . . ?
H51 N5 H52 120.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O2 1.693(3) . ?
Mo1 O1 1.704(2) . ?
Mo1 O3 1.925(2) . ?
Mo1 O4 1.997(2) . ?
Mo1 N1 2.237(3) . ?
Mo1 O5 2.343(2) . ?
O3 C26 1.350(4) . ?
O4 C3 1.318(4) . ?
O5 C11 1.457(4) . ?
N1 C2 1.288(4) . ?
N1 N2 1.401(4) . ?
N2 C3 1.306(4) . ?
C2 C21 1.443(5) . ?
C2 H2 0.927(10) . ?
C3 C31 1.471(5) . ?
C11 C12 1.494(5) . ?
C11 H111 0.971(10) . ?
C11 H112 0.978(10) . ?
C12 H121 0.9600 . ?
C12 H122 0.9600 . ?
C12 H123 0.9600 . ?
C21 C22 1.404(5) . ?
C21 C26 1.409(5) . ?
C22 C23 1.375(6) . ?
C22 H22 0.933(10) . ?
C23 C24 1.375(6) . ?
C23 H23 0.92(5) . ?
C24 C25 1.382(6) . ?
C24 H24 0.924(10) . ?
C25 C26 1.389(5) . ?
C25 H25 0.928(10) . ?
C31 C36 1.401(5) . ?
C31 C32 1.413(5) . ?
C32 C33 1.381(5) . ?
C32 H32 0.928(10) . ?
C33 C34 1.377(6) . ?
C33 H33 0.926(10) . ?
C34 C35 1.379(5) . ?
C34 H34 0.931(10) . ?
C35 C36 1.398(5) . ?
C35 H35 0.934(10) . ?
C36 N5 1.398(4) . ?
N5 H51 0.8600 . ?
N5 H52 0.8600 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Mo1 O3 C26 61.7(3) . . . . ?
O1 Mo1 O3 C26 170.3(3) . . . . ?
O4 Mo1 O3 C26 -59.1(4) . . . . ?
N1 Mo1 O3 C26 -31.0(3) . . . . ?
O5 Mo1 O3 C26 -108.6(3) . . . . ?
O2 Mo1 O4 C3 -91.0(2) . . . . ?
O1 Mo1 O4 C3 161.5(2) . . . . ?
O3 Mo1 O4 C3 29.9(3) . . . . ?
N1 Mo1 O4 C3 0.7(2) . . . . ?
O5 Mo1 O4 C3 79.8(2) . . . . ?
O2 Mo1 O5 C11 155.6(7) . . . . ?
O1 Mo1 O5 C11 -15.6(3) . . . . ?
O3 Mo1 O5 C11 -119.7(3) . . . . ?
O4 Mo1 O5 C11 84.0(3) . . . . ?
N1 Mo1 O5 C11 157.6(3) . . . . ?
O2 Mo1 N1 C2 -79.7(3) . . . . ?
O1 Mo1 N1 C2 119.6(4) . . . . ?
O3 Mo1 N1 C2 18.2(3) . . . . ?
O4 Mo1 N1 C2 -176.7(3) . . . . ?
O5 Mo1 N1 C2 100.6(3) . . . . ?
O2 Mo1 N1 N2 96.4(2) . . . . ?
O1 Mo1 N1 N2 -64.3(4) . . . . ?
O3 Mo1 N1 N2 -165.6(2) . . . . ?
O4 Mo1 N1 N2 -0.6(2) . . . . ?
O5 Mo1 N1 N2 -83.3(2) . . . . ?
C2 N1 N2 C3 177.0(3) . . . . ?
Mo1 N1 N2 C3 0.4(3) . . . . ?
N2 N1 C2 C21 178.5(3) . . . . ?
Mo1 N1 C2 C21 -5.4(5) . . . . ?
N1 N2 C3 O4 0.2(4) . . . . ?
N1 N2 C3 C31 179.3(3) . . . . ?
Mo1 O4 C3 N2 -0.7(4) . . . . ?
Mo1 O4 C3 C31 -179.9(2) . . . . ?
Mo1 O5 C11 C12 -69.7(4) . . . . ?
N1 C2 C21 C22 172.7(4) . . . . ?
N1 C2 C21 C26 -7.6(6) . . . . ?
C26 C21 C22 C23 0.7(6) . . . . ?
C2 C21 C22 C23 -179.6(4) . . . . ?
C21 C22 C23 C24 -0.7(7) . . . . ?
C22 C23 C24 C25 0.3(7) . . . . ?
C23 C24 C25 C26 0.1(6) . . . . ?
Mo1 O3 C26 C25 -152.3(3) . . . . ?
Mo1 O3 C26 C21 29.2(5) . . . . ?
C24 C25 C26 O3 -178.7(3) . . . . ?
C24 C25 C26 C21 -0.2(5) . . . . ?
C22 C21 C26 O3 178.2(3) . . . . ?
C2 C21 C26 O3 -1.5(5) . . . . ?
C22 C21 C26 C25 -0.2(5) . . . . ?
C2 C21 C26 C25 -179.9(3) . . . . ?
N2 C3 C31 C36 20.5(5) . . . . ?
O4 C3 C31 C36 -160.3(3) . . . . ?
N2 C3 C31 C32 -162.0(3) . . . . ?
O4 C3 C31 C32 17.1(4) . . . . ?
C36 C31 C32 C33 -0.8(5) . . . . ?
C3 C31 C32 C33 -178.4(3) . . . . ?
C31 C32 C33 C34 0.1(6) . . . . ?
C32 C33 C34 C35 0.6(6) . . . . ?
C33 C34 C35 C36 -0.6(6) . . . . ?
C34 C35 C36 C31 -0.1(5) . . . . ?
C34 C35 C36 N5 179.6(3) . . . . ?
C32 C31 C36 C35 0.8(5) . . . . ?
C3 C31 C36 C35 178.2(3) . . . . ?
C32 C31 C36 N5 -178.9(3) . . . . ?
C3 C31 C36 N5 -1.5(5) . . . . ?
