#------------------------------------------------------------------------------
#$Date: 2019-11-23 12:06:49 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233220 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/56/7235685.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_7235685
loop_
_publ_author_name
'Chen, Quan-Liang'
'Huang, Wei'
'Chen, Mao-Long'
'Lin, Jing'
'Cao, Ze-Xing'
'Zhou, Zhao-Hui'
_publ_section_title
;
 Transformations and reductions of γ-octamolybdates with their monomeric
 and dimeric amino polycarboxylates
;
_journal_issue                   50
_journal_name_full               'RSC Adv.'
_journal_page_first              26499
_journal_paper_doi               10.1039/C4RA03125C
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'H5 Mo4 N0.5 O15'
_chemical_formula_weight         635.81
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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
_cell_angle_alpha                104.687(10)
_cell_angle_beta                 105.910(10)
_cell_angle_gamma                109.499(10)
_cell_formula_units_Z            2
_cell_length_a                   8.2533(9)
_cell_length_b                   8.3054(10)
_cell_length_c                   10.2054(11)
_cell_measurement_temperature    173(2)
_cell_volume                     586.44(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3454
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    4.263
_exptl_absorpt_correction_T_max  0.8828
_exptl_absorpt_correction_T_min  0.4827
_exptl_crystal_density_diffrn    3.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             593
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2065
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.004
_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          0.0816
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                1666
_reflns_number_total             2065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra03125c2.cif
_cod_data_source_block           mop
_cod_original_cell_volume        586.44(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'H5 Mo4 N0.50 O15'
_cod_database_code               7235685
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 0.27689(9) 0.35210(9) 0.94927(7) 0.00677(19) Uani 1 1 d .
Mo2 Mo 0.41702(9) 0.00268(9) 0.70679(7) 0.00667(19) Uani 1 1 d .
Mo3 Mo 0.27405(8) -0.03897(9) 0.96452(7) 0.00561(18) Uani 1 1 d D
Mo4 Mo 0.44094(9) -0.37922(9) 0.72673(7) 0.00690(19) Uani 1 1 d .
O5 O 0.5039(7) -0.1861(7) 0.6553(6) 0.0097(12) Uani 1 1 d .
O6 O 0.1904(7) -0.1187(7) 0.5767(6) 0.0117(12) Uani 1 1 d .
O1 O 0.4305(7) 0.5205(7) 0.8844(6) 0.0089(12) Uani 1 1 d .
O2 O 0.0485(7) -0.1625(7) 0.8403(6) 0.0127(12) Uani 1 1 d .
O3 O 0.2804(7) 0.1956(7) 1.0698(6) 0.0086(11) Uani 1 1 d .
O4 O 0.4028(7) -0.1466(7) 0.8662(6) 0.0098(12) Uani 1 1 d .
O7 O 0.5210(7) 0.1566(7) 0.6378(6) 0.0112(12) Uani 1 1 d .
O8 O 0.2071(7) -0.5105(8) 0.6139(6) 0.0144(13) Uani 1 1 d .
O9 O 0.2137(7) 0.4905(7) 1.0561(6) 0.0136(12) Uani 1 1 d .
O10 O 0.0805(7) 0.2270(8) 0.7912(6) 0.0151(13) Uani 1 1 d .
O11 O 0.3741(7) 0.1415(7) 0.8593(6) 0.0092(12) Uani 1 1 d .
O12 O 0.5502(7) -0.4917(8) 0.6508(6) 0.0116(12) Uani 1 1 d .
O13 O 0.2893(7) -0.1244(7) 1.1031(6) 0.0093(12) Uani 1 1 d D
H13 H 0.181(4) -0.169(10) 1.109(6) 0.014 Uiso 1 1 d D
N14 N -0.1842(9) -0.1421(9) 0.5806(7) 0.0141(16) Uani 1 1 d G
H14A H -0.1751 -0.2257 0.5190 0.021 Uiso 1 1 d G
H14B H -0.2978 -0.1600 0.5549 0.021 Uiso 1 1 d G
N15 N -0.1271(9) 0.4266(10) 0.6865(8) 0.0149(15) Uani 1 1 d G
H15A H -0.2434 0.3563 0.6523 0.022 Uiso 1 1 d G
H15B H -0.1001 0.3997 0.7622 0.022 Uiso 1 1 d G
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'
N N 0.0061 0.0033 '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
O9 Mo1 O10 103.1(2) . .
O9 Mo1 O1 102.1(2) . .
O10 Mo1 O1 100.1(2) . .
O9 Mo1 O3 94.0(2) . .
O10 Mo1 O3 107.4(3) . .
O1 Mo1 O3 143.9(2) . .
O9 Mo1 O1 93.1(2) . 2_667
O10 Mo1 O1 163.5(2) . 2_667
O1 Mo1 O1 72.9(2) . 2_667
O3 Mo1 O1 74.1(2) . 2_667
O9 Mo1 O11 164.1(2) . .
O10 Mo1 O11 85.2(2) . .
O1 Mo1 O11 89.47(19) . .
O3 Mo1 O11 70.44(19) . .
O1 Mo1 O11 79.81(18) 2_667 .
O7 Mo2 O6 103.2(2) . .
O7 Mo2 O11 105.1(2) . .
O6 Mo2 O11 99.1(2) . .
O7 Mo2 O5 102.6(2) . .
O6 Mo2 O5 98.0(2) . .
O11 Mo2 O5 143.0(2) . .
O7 Mo2 O4 156.3(2) . .
O6 Mo2 O4 100.4(2) . .
O11 Mo2 O4 72.9(2) . .
O5 Mo2 O4 71.87(19) . .
O7 Mo2 O13 86.5(2) . 2_657
O6 Mo2 O13 170.0(2) . 2_657
O11 Mo2 O13 80.8(2) . 2_657
O5 Mo2 O13 76.9(2) . 2_657
O4 Mo2 O13 69.90(18) . 2_657
O7 Mo2 Mo3 144.39(17) . .
O6 Mo2 Mo3 90.78(18) . .
O11 Mo2 Mo3 39.68(16) . .
O5 Mo2 Mo3 107.77(16) . .
O4 Mo2 Mo3 36.23(12) . .
O13 Mo2 Mo3 82.75(13) 2_657 .
O2 Mo3 O13 105.6(3) . .
O2 Mo3 O4 101.8(2) . .
O13 Mo3 O4 100.4(2) . .
O2 Mo3 O3 103.2(2) . .
O13 Mo3 O3 98.3(2) . .
O4 Mo3 O3 143.2(2) . .
O2 Mo3 O11 98.8(2) . .
O13 Mo3 O11 155.5(2) . .
O4 Mo3 O11 75.8(2) . .
O3 Mo3 O11 74.1(2) . .
O2 Mo3 O4 177.0(2) . 2_657
O13 Mo3 O4 77.3(2) . 2_657
O4 Mo3 O4 77.8(2) . 2_657
O3 Mo3 O4 75.83(19) . 2_657
O11 Mo3 O4 78.21(19) . 2_657
O2 Mo3 Mo2 91.08(19) . .
O13 Mo3 Mo2 144.39(16) . .
O4 Mo3 Mo2 44.64(15) . .
O3 Mo3 Mo2 108.35(15) . .
O11 Mo3 Mo2 34.26(13) . .
O4 Mo3 Mo2 86.60(12) 2_657 .
O12 Mo4 O8 104.2(3) . .
O12 Mo4 O5 96.3(2) . .
O8 Mo4 O5 101.3(2) . .
O12 Mo4 O1 98.9(2) . 1_545
O8 Mo4 O1 95.4(2) . 1_545
O5 Mo4 O1 154.0(2) . 1_545
O12 Mo4 O4 159.0(2) . .
O8 Mo4 O4 95.8(2) . .
O5 Mo4 O4 73.2(2) . .
O1 Mo4 O4 85.42(19) 1_545 .
O12 Mo4 O3 89.0(2) . 2_657
O8 Mo4 O3 163.4(2) . 2_657
O5 Mo4 O3 87.0(2) . 2_657
O1 Mo4 O3 72.3(2) 1_545 2_657
O4 Mo4 O3 72.56(17) . 2_657
Mo4 O5 Mo2 117.8(3) . .
Mo1 O1 Mo4 146.6(3) . 1_565
Mo1 O1 Mo1 107.1(2) . 2_667
Mo4 O1 Mo1 106.2(2) 1_565 2_667
Mo3 O3 Mo1 112.3(2) . .
Mo3 O3 Mo4 111.5(2) . 2_657
Mo1 O3 Mo4 102.9(2) . 2_657
Mo3 O4 Mo4 155.4(3) . .
Mo3 O4 Mo2 99.1(2) . .
Mo4 O4 Mo2 92.89(19) . .
Mo3 O4 Mo3 102.2(2) . 2_657
Mo4 O4 Mo3 97.83(17) . 2_657
Mo2 O4 Mo3 95.44(19) . 2_657
Mo2 O11 Mo3 106.1(2) . .
Mo2 O11 Mo1 151.3(3) . .
Mo3 O11 Mo1 96.88(19) . .
Mo3 O13 Mo2 117.1(3) . 2_657
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O9 1.691(5) .
Mo1 O10 1.703(5) .
Mo1 O1 1.936(5) .
Mo1 O3 2.005(5) .
Mo1 O1 2.229(5) 2_667
Mo1 O11 2.252(5) .
Mo2 O7 1.709(5) .
Mo2 O6 1.726(5) .
Mo2 O11 1.882(5) .
Mo2 O5 1.946(5) .
Mo2 O4 2.286(5) .
Mo2 O13 2.335(5) 2_657
Mo2 Mo3 3.2126(10) .
Mo3 O2 1.702(5) .
Mo3 O13 1.729(5) .
Mo3 O4 1.923(5) .
Mo3 O3 1.947(5) .
Mo3 O11 2.135(5) .
Mo3 O4 2.419(5) 2_657
Mo4 O12 1.693(5) .
Mo4 O8 1.726(5) .
Mo4 O5 1.902(5) .
Mo4 O1 1.999(5) 1_545
Mo4 O4 2.262(5) .
Mo4 O3 2.316(5) 2_657
O1 Mo4 1.999(5) 1_565
O1 Mo1 2.229(5) 2_667
O3 Mo4 2.316(5) 2_657
O4 Mo3 2.419(5) 2_657
O13 Mo2 2.335(5) 2_657
