#------------------------------------------------------------------------------
#$Date: 2016-03-19 08:29:54 +0100 (Sat 19 de Mar de 2016) $
#$Revision: 178363 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/46/7224647.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_7224647
loop_
_publ_author_name
'Najafi, Mahnaz'
'Abbasi, Alireza'
'Masteri-Farahani, Majid'
'Shahbaazi, Hamidreza'
'Ahmadniai Motlagh, Mahmood'
'Janczak, Jan'
_publ_section_title
;
 A one-dimensional polyoxomolybdate polymer as catalyst for the
 epoxidation of olefins
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA02248K
_journal_year                    2016
_chemical_formula_moiety         'Mo4 O13, 2(H4 N)'
_chemical_formula_sum            'H8 Mo4 N2 O13'
_chemical_formula_weight         627.84
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-11-04 deposited with the CCDC.
2016-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                104.702(5)
_cell_angle_beta                 106.043(4)
_cell_angle_gamma                109.624(6)
_cell_formula_units_Z            2
_cell_length_a                   8.2674(4)
_cell_length_b                   8.3564(4)
_cell_length_c                   10.2593(5)
_cell_measurement_reflns_used    2330
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.84
_cell_volume                     592.71(7)
_computing_cell_refinement
;
Oxford Diffraction Poland (2008). CrysAlis Red, Version 171.32.6
;
_computing_data_collection
;
Oxford Diffraction Poland (2008). CrysAlis CCD, Version 171.32.6
;
_computing_data_reduction
;
Oxford Diffraction Poland (2008). CrysAlis Red, Version 171.32.6
;
_computing_molecular_graphics
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'KUMA KM-4 with CCD detector'
_diffrn_measurement_method       ω-scan
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7192
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    4.207
_exptl_absorpt_correction_T_max  0.7317
_exptl_absorpt_correction_T_min  0.4665
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Oxford Diffraction Poland (2008). CrysAlis Red, Version 171.32.6
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    3.518
_exptl_crystal_density_meas      3.515
_exptl_crystal_density_method    piknometric
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2945
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0275
_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)+(0.0268P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                2330
_reflns_number_total             2945
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c6ra02248k2.cif
_cod_data_source_block           mn8
_cod_database_code               7224647
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mo1 Mo 0.08189(5) 0.49795(5) 0.29252(4) 0.01290(9) Uani 1 1 d .
Mo2 Mo 0.05812(5) 0.87841(5) 0.27193(4) 0.01307(9) Uani 1 1 d .
Mo3 Mo -0.22350(5) 0.85031(5) -0.05302(4) 0.01300(9) Uani 1 1 d .
Mo4 Mo -0.22674(5) 0.46035(5) -0.03695(4) 0.01153(9) Uani 1 1 d .
O1 O 0.3077(4) 0.6196(4) 0.4226(3) 0.0208(7) Uani 1 1 d .
O2 O -0.4523(4) 0.3360(4) -0.1622(3) 0.0199(7) Uani 1 1 d .
O3 O 0.2906(4) 1.0078(4) 0.3826(3) 0.0237(7) Uani 1 1 d .
O4 O -0.2896(4) 0.9869(4) 0.0507(4) 0.0261(7) Uani 1 1 d .
O5 O -0.2144(4) 0.3753(4) 0.1012(3) 0.0167(6) Uani 1 1 d .
O6 O 0.0986(4) 0.6482(4) 0.1335(3) 0.0140(6) Uani 1 1 d .
O7 O 0.0686(4) 0.9797(4) 0.1159(3) 0.0150(6) Uani 1 1 d .
O8 O -0.0046(4) 0.6873(4) 0.3440(3) 0.0165(6) Uani 1 1 d .
O9 O -0.2205(4) 0.6946(4) 0.0686(3) 0.0133(6) Uani 1 1 d .
O10 O 0.1246(4) 0.3588(4) 0.1403(3) 0.0133(6) Uani 1 1 d .
O11 O -0.0224(4) 0.3453(4) 0.3603(3) 0.0219(7) Uani 1 1 d .
O12 O -0.4194(4) 0.7235(4) -0.2122(4) 0.0252(7) Uani 1 1 d .
O13 O -0.0496(4) 0.9908(4) 0.3485(3) 0.0220(7) Uani 1 1 d .
N1 N 0.3724(5) 0.9251(5) 0.6893(5) 0.0297(10) Uani 1 1 d D
H11 H 0.407(5) 0.905(5) 0.619(3) 0.045 Uiso 1 1 d D
H12 H 0.421(5) 0.888(5) 0.752(3) 0.045 Uiso 1 1 d D
H13 H 0.406(5) 1.0391(13) 0.729(4) 0.045 Uiso 1 1 d D
H14 H 0.2543(9) 0.868(4) 0.657(4) 0.045 Uiso 1 1 d D
N2 N 0.3148(5) 0.3563(5) 0.5794(4) 0.0248(9) Uani 1 1 d D
H21 H 0.346(5) 0.459(2) 0.571(4) 0.037 Uiso 1 1 d D
H22 H 0.2005(15) 0.310(4) 0.565(4) 0.037 Uiso 1 1 d D
H23 H 0.380(4) 0.371(5) 0.6649(16) 0.037 Uiso 1 1 d D
H24 H 0.334(5) 0.285(4) 0.517(3) 0.037 Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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
O11 Mo1 O1 103.27(14) . .
O11 Mo1 O10 105.00(13) . .
O1 Mo1 O10 99.30(13) . .
O11 Mo1 O8 102.60(13) . .
O1 Mo1 O8 97.70(13) . .
O10 Mo1 O8 143.08(11) . .
O11 Mo1 O6 156.60(13) . .
O1 Mo1 O6 100.03(12) . .
O10 Mo1 O6 72.96(10) . .
O8 Mo1 O6 71.94(10) . .
O11 Mo1 O5 86.32(13) . .
O1 Mo1 O5 169.92(11) . .
O10 Mo1 O5 80.86(11) . .
O8 Mo1 O5 76.92(11) . .
O6 Mo1 O5 70.29(9) . .
O11 Mo1 Mo4 144.39(11) . 2_565
O1 Mo1 Mo4 90.68(10) . 2_565
O10 Mo1 Mo4 39.76(8) . 2_565
O8 Mo1 Mo4 107.83(8) . 2_565
O6 Mo1 Mo4 36.21(7) . 2_565
O5 Mo1 Mo4 83.02(7) . 2_565
O13 Mo2 O3 104.22(15) . .
O13 Mo2 O8 95.97(13) . .
O3 Mo2 O8 101.29(13) . .
O13 Mo2 O7 98.72(12) . .
O3 Mo2 O7 94.95(13) . .
O8 Mo2 O7 154.69(12) . .
O13 Mo2 O6 159.80(13) . .
O3 Mo2 O6 94.96(13) . .
O8 Mo2 O6 73.76(10) . .
O7 Mo2 O6 85.70(10) . .
O13 Mo2 O9 89.60(13) . .
O3 Mo2 O9 162.78(12) . .
O8 Mo2 O9 87.17(11) . .
O7 Mo2 O9 72.49(10) . .
O6 Mo2 O9 72.84(10) . .
O4 Mo3 O12 102.94(16) . .
O4 Mo3 O7 101.69(13) . 2_575
O12 Mo3 O7 100.31(13) . 2_575
O4 Mo3 O9 94.19(13) . .
O12 Mo3 O9 107.39(13) . .
O7 Mo3 O9 143.98(11) 2_575 .
O4 Mo3 O7 93.21(13) . .
O12 Mo3 O7 163.56(13) . .
O7 Mo3 O7 73.05(12) 2_575 .
O9 Mo3 O7 73.96(10) . .
O4 Mo3 O10 164.30(12) . 2_565
O12 Mo3 O10 85.04(13) . 2_565
O7 Mo3 O10 89.95(10) 2_575 2_565
O9 Mo3 O10 70.38(10) . 2_565
O7 Mo3 O10 80.01(10) . 2_565
O2 Mo4 O5 105.20(13) . .
O2 Mo4 O6 101.42(13) . 2_565
O5 Mo4 O6 100.49(12) . 2_565
O2 Mo4 O9 103.48(13) . .
O5 Mo4 O9 97.88(12) . .
O6 Mo4 O9 143.78(11) 2_565 .
O2 Mo4 O10 99.06(12) . 2_565
O5 Mo4 O10 155.65(12) . 2_565
O6 Mo4 O10 76.32(11) 2_565 2_565
O9 Mo4 O10 74.13(10) . 2_565
O2 Mo4 O6 176.75(11) . .
O5 Mo4 O6 78.05(11) . .
O6 Mo4 O6 77.98(12) 2_565 .
O9 Mo4 O6 75.66(10) . .
O10 Mo4 O6 77.68(10) 2_565 .
O2 Mo4 Mo1 90.97(10) . 2_565
O5 Mo4 Mo1 144.87(9) . 2_565
O6 Mo4 Mo1 45.03(8) 2_565 2_565
O9 Mo4 Mo1 108.55(8) . 2_565
O10 Mo4 Mo1 34.42(7) 2_565 2_565
O6 Mo4 Mo1 86.37(6) . 2_565
Mo4 O5 Mo1 116.55(13) . .
Mo4 O6 Mo2 156.29(14) 2_565 .
Mo4 O6 Mo1 98.76(11) 2_565 .
Mo2 O6 Mo1 92.68(10) . .
Mo4 O6 Mo4 102.02(12) 2_565 .
Mo2 O6 Mo4 97.58(10) . .
Mo1 O6 Mo4 94.90(9) . .
Mo3 O7 Mo2 146.43(16) 2_575 .
Mo3 O7 Mo3 106.95(12) 2_575 .
Mo2 O7 Mo3 106.56(11) . .
Mo2 O8 Mo1 117.72(14) . .
Mo4 O9 Mo3 111.91(13) . .
Mo4 O9 Mo2 111.59(12) . .
Mo3 O9 Mo2 102.96(11) . .
Mo1 O10 Mo4 105.82(12) . 2_565
Mo1 O10 Mo3 150.92(14) . 2_565
Mo4 O10 Mo3 97.10(10) 2_565 2_565
H11 N1 H12 109.8(8) . .
H11 N1 H13 109.6(8) . .
H12 N1 H13 109.6(8) . .
H11 N1 H14 109.5(8) . .
H12 N1 H14 109.2(8) . .
H13 N1 H14 109.2(8) . .
H21 N2 H22 109.7(8) . .
H21 N2 H23 109.3(8) . .
H22 N2 H23 109.7(8) . .
H21 N2 H24 109.5(8) . .
H22 N2 H24 109.6(8) . .
H23 N2 H24 109.1(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O11 1.702(3) .
Mo1 O1 1.720(3) .
Mo1 O10 1.890(3) .
Mo1 O8 1.959(3) .
Mo1 O6 2.303(3) .
Mo1 O5 2.353(3) .
Mo1 Mo4 3.2170(5) 2_565
Mo2 O13 1.693(3) .
Mo2 O3 1.711(3) .
Mo2 O8 1.903(3) .
Mo2 O7 2.001(3) .
Mo2 O6 2.266(3) .
Mo2 O9 2.315(3) .
Mo3 O4 1.690(3) .
Mo3 O12 1.709(3) .
Mo3 O7 1.942(3) 2_575
Mo3 O9 2.020(2) .
Mo3 O7 2.233(3) .
Mo3 O10 2.257(3) 2_565
Mo4 O2 1.704(3) .
Mo4 O5 1.734(3) .
Mo4 O6 1.923(3) 2_565
Mo4 O9 1.957(3) .
Mo4 O10 2.138(3) 2_565
Mo4 O6 2.435(3) .
Mo4 Mo1 3.2170(5) 2_565
O6 Mo4 1.923(3) 2_565
O7 Mo3 1.942(3) 2_575
O10 Mo4 2.138(3) 2_565
O10 Mo3 2.257(3) 2_565
N1 H11 0.844(5) .
N1 H12 0.844(5) .
N1 H13 0.845(5) .
N1 H14 0.847(5) .
N2 H21 0.845(5) .
N2 H22 0.844(5) .
N2 H23 0.846(5) .
N2 H24 0.846(5) .
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
N1 H11 O3 0.844(5) 2.36(3) 2.986(5) 131(3) 2_676 y
N1 H11 O1 0.844(5) 2.40(3) 3.003(5) 129(3) . y
N1 H12 O12 0.844(5) 2.23(2) 2.945(5) 143(3) 1_656 y
N1 H13 O2 0.845(5) 2.17(2) 2.999(5) 168(3) 1_666 y
N1 H14 O11 0.847(5) 2.06(2) 2.819(5) 149(3) 2_566 y
N1 H14 O13 0.847(5) 2.36(3) 2.931(5) 125(3) 2_576 y
N2 H21 O1 0.845(5) 2.30(2) 3.043(5) 148(3) . y
N2 H21 O12 0.845(5) 2.42(3) 2.891(5) 116(3) 1_656 y
N2 H22 O8 0.844(5) 2.09(2) 2.821(5) 145(3) 2_566 y
N2 H22 O11 0.844(5) 2.53(3) 3.015(5) 117(3) . y
N2 H23 O2 0.846(5) 2.08(2) 2.897(5) 162(3) 1_656 y
N2 H24 O3 0.846(5) 2.22(2) 3.000(5) 153(3) 1_545 y
