#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:58:48 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179402 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329973.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_4329973
loop_
_publ_author_name
'Sónia Figueiredo'
'Ana C. Gomes'
'Patrícia Neves'
'Tatiana R. Amarante'
'Filipe A. Almeida Paz'
'Rosário Soares'
'André D. Lopes'
'Anabela A. Valente'
'Martyn Pillinger'
'Isabel S. Gonçalves'
_publ_contact_author_address
; Department of Chemistry
  University of Aveiro
  CICECO
  3810-193
  Aveiro
  Portugal
;
_publ_contact_author_email       igoncalves@ua.pt
_publ_contact_author_fax         '+351 234 370084'
_publ_contact_author_name        'Professor Isabel S. Goncalves'
_publ_contact_author_phone       '+351 234 370200'
_publ_section_title
;
 Synthesis, Structural Elucidation, and Application of a
 Pyrazolylpyridine-Molybdenum Oxide Composite as a Heterogeneous Catalyst
 for Olefin Epoxidation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8629
_journal_page_last               8635
_journal_paper_doi               10.1021/ic301405r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C10 H9 Mo2 N3 O8'
_chemical_formula_sum            'C10 H9 Mo2 N3 O8'
_chemical_formula_weight         491.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             '01 February 2012'
_audit_creation_method           'Manual editing plus fullprof.2k'
_cell_angle_alpha                99.0733(15)
_cell_angle_beta                 93.715(4)
_cell_angle_gamma                97.954(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4022(3)
_cell_length_b                   8.5156(4)
_cell_length_c                   11.2499(5)
_cell_measurement_temperature    298
_cell_volume                     690.79(5)
_computing_molecular_graphics    'Crystal Impact Diamond 3.1f'
_computing_structure_refinement  FULLPROF
_computing_structure_solution    eXpo2004
_diffrn_ambient_temperature      298
_diffrn_detector_type            'X Celerator detector'
_diffrn_measurement_device_type  'PANalaytical X'Pert Pro'
_diffrn_measurement_method       Bragg-Brentano
_diffrn_radiation_monochromator  none
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'x-ray tube'
_diffrn_source_target            'Cu K\a'
_exptl_crystal_density_diffrn    2.361
_pd_char_colour                  White
_pd_instr_location
; 
Conventional powder diffractometer instrument belonging to the 
University of Aveiro and located at the Central Analytical Laboratory
;
_pd_meas_2theta_range_inc        0.020054
_pd_meas_2theta_range_max        99.99310
_pd_meas_2theta_range_min        6.00000
_pd_meas_number_of_points        4688
_pd_meas_scan_method             cont
_pd_proc_2theta_range_inc        0.020054
_pd_proc_2theta_range_max        100.0245
_pd_proc_2theta_range_min        6.0314
_pd_proc_ls_background_function  'Fixed Points'
_pd_proc_ls_pref_orient_corr
; 
 none
;
_pd_proc_ls_profile_function     Pseudo-Voigt
_pd_proc_ls_prof_R_factor        4.6763
_pd_proc_ls_prof_wR_expected     3.0722
_pd_proc_ls_prof_wR_factor       6.0975
_pd_proc_wavelength              1.540560
_pd_spec_mounting
; 
 Glass slide
;
_pd_spec_mount_mode              Reflection
_pd_spec_shape                   'Flat sheet'
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     86
_refine_ls_number_reflns         3044
_refine_ls_number_restraints     4
_refine_ls_R_I_factor            7.9299
_cod_data_source_file            ic301405r_si_003.cif
_cod_data_source_block           2
_cod_database_code               4329973
#BEGIN Tags that were not found in dictionaries:
_pd_proc_ls_prof_cr_factor       14.2878
_pd_proc_ls_prof_cwr_factor      13.0663
_pd_proc_ls_prof_cwr_expected    6.5834
_pd_proc_ls_prof_chi2            3.9392
_pd_proc_ls_prof_echi2           4.0004
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_type_symbol
Mo1 0.3997(10) 0.0689(6) 0.6230(5) 0.0557(9) 1.00000 Uiso Mo
Mo2 0.0938(10) -0.1113(7) 0.3920(5) 0.0557(9) 1.00000 Uiso Mo
O1 0.354(5) -0.085(4) 0.421(3) 0.029(4) 1.00000 Uiso O
O2 0.417(4) -0.090(2) 0.6984(20) 0.029(4) 1.00000 Uiso O
O3 0.440(5) 0.201(3) 0.7535(17) 0.029(4) 1.00000 Uiso O
O4 0.032(4) -0.2923(19) 0.433(2) 0.029(4) 1.00000 Uiso O
O5 0.097(5) -0.168(4) 0.2424(10) 0.029(4) 1.00000 Uiso O
O6 -0.135(5) -0.027(4) 0.415(3) 0.029(4) 1.00000 Uiso O
O7 0.384(5) 0.252(4) 0.520(3) 0.029(4) 1.00000 Uiso O
O8 0.180(5) 0.139(4) 0.371(3) 0.029(4) 1.00000 Uiso O
C1 0.303(8) 0.250(5) 0.420(5) 0.035(5) 1.00000 Uiso C
C2 0.353(8) 0.382(7) 0.345(4) 0.035(5) 1.00000 Uiso C
H2A 0.48333 0.41428 0.36038 0.02533 1.00000 Uiso H
H2B 0.29739 0.47178 0.37873 0.02533 1.00000 Uiso H
N1 0.312(6) 0.359(6) 0.216(4) 0.035(5) 1.00000 Uiso N
N2 0.262(7) 0.485(5) 0.169(5) 0.035(5) 1.00000 Uiso N
N3 0.184(6) 0.701(6) 0.005(4) 0.035(5) 1.00000 Uiso N
H3 0.18825 0.73910 0.08462 0.02533 1.00000 Uiso H
C3 0.349(8) 0.238(7) 0.133(5) 0.035(5) 1.00000 Uiso C
H3A 0.38130 0.13669 0.14684 0.02533 1.00000 Uiso H
C4 0.331(8) 0.287(7) 0.022(5) 0.035(5) 1.00000 Uiso C
H4 0.35907 0.23495 -0.05476 0.02533 1.00000 Uiso H
C5 0.263(8) 0.436(8) 0.050(6) 0.035(5) 1.00000 Uiso C
C6 0.217(8) 0.543(8) -0.034(6) 0.035(5) 1.00000 Uiso C
C7 0.144(8) 0.798(6) -0.078(5) 0.035(5) 1.00000 Uiso C
H7 0.12186 0.90576 -0.05147 0.02533 1.00000 Uiso H
C8 0.137(7) 0.738(7) -0.200(5) 0.035(5) 1.00000 Uiso C
H8 0.11014 0.80359 -0.25870 0.02533 1.00000 Uiso H
C9 0.170(9) 0.580(7) -0.239(5) 0.035(5) 1.00000 Uiso C
H9 0.16487 0.53880 -0.32410 0.02533 1.00000 Uiso H
C10 0.209(8) 0.483(6) -0.156(6) 0.035(5) 1.00000 Uiso C
H10 0.23157 0.37469 -0.18270 0.02533 1.00000 Uiso H
loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
MO 3.70250 0.27720 17.23560 1.09580 12.88760 11.00400 3.74290 61.65840 4.38750
-0.19100 2.73500
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.04700 0.03200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.01700 0.00900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304
0.00000 0.00000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900
0.02900 0.01800
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
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
O1 Mo1 O2 96.9(11) . . yes
O1 Mo1 O3 171.2(12) . . yes
O1 Mo1 O7 79.1(12) . . yes
O1 Mo1 O6 75.0(13) . 2_556 yes
O1 Mo1 O1 79.1(14) . 2_656 yes
O2 Mo1 O3 91.5(11) . . yes
O2 Mo1 O7 175.7(13) . . yes
O2 Mo1 O6 97.3(14) . 2_556 yes
O1 Mo1 O2 94.4(14) 2_656 . yes
O3 Mo1 O7 92.4(12) . . yes
O3 Mo1 O6 106.6(16) . 2_556 yes
O1 Mo1 O3 97.6(16) 2_656 . yes
O6 Mo1 O7 83.3(14) 2_556 . yes
O1 Mo1 O7 83.4(15) 2_656 . yes
O1 Mo1 O6 152.7(14) 2_656 2_556 yes
O1 Mo2 O4 101.4(15) . . yes
O1 Mo2 O5 93.4(16) . . yes
O1 Mo2 O6 149.5(15) . . yes
O1 Mo2 O8 76.8(14) . . yes
O1 Mo2 O6 79.1(14) . 2_556 yes
O4 Mo2 O5 100.0(14) . . yes
O4 Mo2 O6 98.0(15) . . yes
O4 Mo2 O8 170.5(12) . . yes
O4 Mo2 O6 94.7(12) . 2_556 yes
O5 Mo2 O6 106.2(16) . . yes
O5 Mo2 O8 89.4(15) . . yes
O5 Mo2 O6 164.6(15) . 2_556 yes
O6 Mo2 O8 80.2(14) . . yes
O6 Mo2 O6 76.0(14) . 2_556 yes
O6 Mo2 O8 75.8(12) 2_556 . yes
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 O1 2.42(3) . yes
Mo1 O2 1.72(2) . yes
Mo1 O3 1.69(2) . yes
Mo1 O6 1.95(4) 2_556 yes
Mo1 O7 2.10(3) . yes
Mo1 O1 1.91(4) 2_656 yes
Mo2 O1 1.91(4) . yes
Mo2 O4 1.689(18) . yes
Mo2 O5 1.679(14) . yes
Mo2 O6 1.95(4) . yes
Mo2 O6 2.28(3) 2_556 yes
Mo2 O8 2.19(3) . yes
O7 C1 1.24(6) . yes
O8 C1 1.25(6) . yes
N1 N2 1.35(7) . yes
N1 C2 1.44(6) . yes
N1 C3 1.35(7) . yes
N2 C5 1.34(9) . yes
N3 C6 1.41(8) . yes
N3 C7 1.39(7) . yes
N3 H3 0.9000 . no
C1 C2 1.53(7) . no
C3 C4 1.38(8) . no
C4 C5 1.43(9) . no
C5 C6 1.47(9) . no
C6 C10 1.38(9) . no
C7 C8 1.38(8) . no
C8 C9 1.41(8) . no
C9 C10 1.38(8) . no
C2 H2A 0.9600 . no
C2 H2B 0.9600 . no
C3 H3A 0.9600 . no
C4 H4 0.9600 . no
C7 H7 0.9600 . no
C8 H8 0.9600 . no
C9 H9 0.9600 . no
C10 H10 0.9600 . no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O5 0.9000 2.0200 2.88(5) 158 1_565 yes
C3 H3A O2 0.9600 2.3400 3.02(6) 128 2_656 yes
C4 H4 O3 0.9600 2.2600 3.18(6) 160 1_554 yes
C8 H8 O2 0.9600 2.4400 2.79(6) 101 1_564 yes
C8 H8 O8 0.9600 2.5700 3.32(7) 136 2_565 yes
C9 H9 O4 0.9600 2.4800 3.14(6) 126 2_555 yes
C10 H10 O3 0.9600 2.3500 3.21(6) 148 1_554 yes
