#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176809 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/04/2240416.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2240416
loop_
_publ_author_name
'Parimala, Sowmianarayanan'
'Selvam, Parasuraman'
_publ_section_title
;
 Crystal structure of
 aquadioxido(2-{[(2-oxidoethyl)imino]methyl}phenolato-κ³O,N,O')molybdenum(VI)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m35
_journal_page_last               m36
_journal_paper_doi               10.1107/S2056989015001231
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Mo (C9 H9 N O2) O2 (H2 O)]'
_chemical_formula_moiety         'C9 H11 Mo N O5'
_chemical_formula_sum            'C9 H11 Mo N O5'
_chemical_formula_weight         309.13
_chemical_name_systematic
Aquadioxido(2-{[(2-oxidoethyl)imino]methyl}phenolato-κ³O,N,O')molybdenum(VI)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 99.4860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9710(3)
_cell_length_b                   6.70260(10)
_cell_length_c                   10.8673(2)
_cell_measurement_reflns_used    6907
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.76
_cell_volume                     1075.56(3)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0119
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.224
_diffrn_reflns_theta_min         1.379
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.9342
_exptl_absorpt_correction_T_min  0.8126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0162
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0163P)²+0.8254P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0422
_reflns_number_gt                2263
_reflns_number_total             2392
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm5114sup1.cf
_cod_data_source_block           I
_cod_database_code               2240416
_cod_database_fobs_code          2240416
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelx_estimated_absorpt_t_min   0.749
_shelx_estimated_absorpt_t_max   0.887
_shelxl_version_number           .000002012
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
C C1 0.37800(15) -0.3126(3) 0.4461(2) 0.0394(5) Uani d 1
H H1A 0.3281 -0.3758 0.4778 0.047 Uiso calc 1
H H1B 0.4281 -0.4060 0.4541 0.047 Uiso calc 1
C C2 0.34936(14) -0.2553(3) 0.31132(19) 0.0384(5) Uani d 1
H H2A 0.4018 -0.2223 0.2734 0.046 Uiso calc 1
H H2B 0.3169 -0.3641 0.2649 0.046 Uiso calc 1
C C3 0.22629(12) -0.0467(3) 0.22157(16) 0.0288(4) Uani d 1
H H3 0.2174 -0.1379 0.1562 0.035 Uiso calc 1
C C4 0.16677(11) 0.1238(3) 0.21392(16) 0.0267(4) Uani d 1
C C5 0.09354(13) 0.1343(3) 0.11473(18) 0.0371(4) Uani d 1
H H5 0.0846 0.0313 0.0567 0.044 Uiso calc 1
C C6 0.03507(13) 0.2930(4) 0.10178(19) 0.0427(5) Uani d 1
H H6 -0.0136 0.2961 0.0365 0.051 Uiso calc 1
C C7 0.04887(13) 0.4486(4) 0.1865(2) 0.0404(5) Uani d 1
H H7 0.0090 0.5561 0.1780 0.049 Uiso calc 1
C C8 0.12118(13) 0.4458(3) 0.28334(18) 0.0331(4) Uani d 1
H H8 0.1304 0.5525 0.3387 0.040 Uiso calc 1
C C9 0.18051(11) 0.2837(3) 0.29870(15) 0.0244(3) Uani d 1
Mo Mo1 0.32157(2) 0.08935(2) 0.49415(2) 0.02134(5) Uani d 1
N N1 0.29025(10) -0.0807(2) 0.31202(14) 0.0254(3) Uani d 1
O O1 0.40476(8) -0.13539(19) 0.51476(12) 0.0286(3) Uani d 1
O O2 0.25056(8) 0.29088(18) 0.39282(11) 0.0275(3) Uani d 1
O O3 0.42590(10) 0.2153(2) 0.37755(13) 0.0306(3) Uani d 1
O O4 0.37757(10) 0.2275(2) 0.61586(12) 0.0372(3) Uani d 1
O O5 0.23417(9) -0.0248(2) 0.54594(13) 0.0392(3) Uani d 1
H H1O 0.4715(17) 0.176(4) 0.395(2) 0.037(7) Uiso d 1
H H2O 0.4144(17) 0.221(4) 0.305(3) 0.048(7) Uiso d 1
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
O1 C1 C2 107.86(16)
O1 C1 H1A 110.1
C2 C1 H1A 110.1
O1 C1 H1B 110.1
C2 C1 H1B 110.1
H1A C1 H1B 108.4
N1 C2 C1 105.88(15)
N1 C2 H2A 110.6
C1 C2 H2A 110.6
N1 C2 H2B 110.6
C1 C2 H2B 110.6
H2A C2 H2B 108.7
N1 C3 C4 124.35(16)
N1 C3 H3 117.8
C4 C3 H3 117.8
C9 C4 C5 118.37(17)
C9 C4 C3 122.93(15)
C5 C4 C3 118.66(17)
C6 C5 C4 121.4(2)
C6 C5 H5 119.3
C4 C5 H5 119.3
C5 C6 C7 119.60(18)
C5 C6 H6 120.2
C7 C6 H6 120.2
C8 C7 C6 120.62(19)
C8 C7 H7 119.7
C6 C7 H7 119.7
C7 C8 C9 120.37(19)
C7 C8 H8 119.8
C9 C8 H8 119.8
O2 C9 C8 117.79(16)
O2 C9 C4 122.62(15)
C8 C9 C4 119.56(16)
O5 Mo1 O4 107.11(7)
O5 Mo1 O1 97.32(6)
O4 Mo1 O1 96.15(6)
O5 Mo1 O2 97.01(6)
O4 Mo1 O2 102.33(6)
O1 Mo1 O2 152.09(5)
O5 Mo1 N1 90.18(6)
O4 Mo1 N1 161.73(6)
O1 Mo1 N1 75.35(5)
O2 Mo1 N1 80.78(5)
O5 Mo1 O3 166.38(6)
O4 Mo1 O3 86.41(6)
O1 Mo1 O3 82.47(5)
O2 Mo1 O3 78.05(5)
N1 Mo1 O3 76.56(5)
C3 N1 C2 121.04(15)
C3 N1 Mo1 127.21(12)
C2 N1 Mo1 111.56(11)
C1 O1 Mo1 117.80(11)
C9 O2 Mo1 133.92(11)
Mo1 O3 H1O 114.5(19)
Mo1 O3 H2O 120.8(18)
H1O O3 H2O 109(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 1.425(2) ?
C1 C2 1.507(3) ?
C1 H1A 0.9700 ?
C1 H1B 0.9700 ?
C2 N1 1.468(2) ?
C2 H2A 0.9700 ?
C2 H2B 0.9700 ?
C3 N1 1.275(2) ?
C3 C4 1.443(3) ?
C3 H3 0.9300 ?
C4 C9 1.406(3) ?
C4 C5 1.407(2) ?
C5 C6 1.370(3) ?
C5 H5 0.9300 ?
C6 C7 1.384(3) ?
C6 H6 0.9300 ?
C7 C8 1.380(3) ?
C7 H7 0.9300 ?
C8 C9 1.396(2) ?
C8 H8 0.9300 ?
C9 O2 1.3397(19) ?
Mo1 O5 1.6902(14) y
Mo1 O4 1.7160(13) y
Mo1 O1 1.9438(12) y
Mo1 O2 1.9446(12) y
Mo1 N1 2.2652(14) y
Mo1 O3 2.3259(14) y
O3 H1O 0.73(2) ?
O3 H2O 0.78(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H1O O1 3_656 0.73(2) 1.97(3) 2.6656(19) 161(3)
O3 H2O O4 4_565 0.78(3) 2.07(3) 2.8425(19) 173(3)
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
O1 C1 C2 N1 -46.2(2)
N1 C3 C4 C9 8.2(3)
N1 C3 C4 C5 -174.14(18)
C9 C4 C5 C6 -1.7(3)
C3 C4 C5 C6 -179.50(19)
C4 C5 C6 C7 1.2(3)
C5 C6 C7 C8 0.3(3)
C6 C7 C8 C9 -1.3(3)
C7 C8 C9 O2 178.67(17)
C7 C8 C9 C4 0.7(3)
C5 C4 C9 O2 -177.10(16)
C3 C4 C9 O2 0.6(3)
C5 C4 C9 C8 0.8(3)
C3 C4 C9 C8 178.44(16)
C4 C3 N1 C2 -178.44(18)
C4 C3 N1 Mo1 7.0(3)
C1 C2 N1 C3 -149.68(18)
C1 C2 N1 Mo1 25.66(19)
C2 C1 O1 Mo1 51.2(2)
C8 C9 O2 Mo1 152.01(14)
C4 C9 O2 Mo1 -30.1(2)
