#------------------------------------------------------------------------------
#$Date: 2019-11-23 22:21:54 +0200 (Sat, 23 Nov 2019) $
#$Revision: 235347 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/62/7236276.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_7236276
loop_
_publ_author_name
'Zhao, Y. H.'
'Jin, X. C.'
'Chen, L.'
'Ding, Y. F.'
'Mao, Z.'
'Fu, H.'
'Ao, Y. H.'
_publ_section_title
;
 Two new molybdates based on ∞ [MonO3n+1]2− units (n = 11, 4)
 with proton conduction under ionothermal
;
_journal_issue                   12
_journal_name_full               'RSC Advances'
_journal_page_first              7210
_journal_paper_doi               10.1039/C6RA26729G
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C13 H16 Mo4 N2 O13'
_chemical_formula_weight         792.04
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-12-22 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.929(2)
_cell_length_b                   9.7226(19)
_cell_length_c                   19.633(4)
_cell_measurement_reflns_used    19051
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.125
_cell_volume                     2041.9(7)
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       'φ and 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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15506
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.473
_exptl_absorpt_correction_T_max  0.6376
_exptl_absorpt_correction_T_min  0.5242
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.565
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       shelxl
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0696P)²+2.3300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                3392
_reflns_number_total             3588
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra26729g2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2041.8(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7236276
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Mo1 Mo 0.07218(3) 0.69558(3) 0.065242(15) 0.01406(11) Uani 1 1 d .
Mo2 Mo -0.17729(3) 0.66748(3) -0.071961(16) 0.01594(11) Uani 1 1 d .
Mo3 Mo 0.25847(3) 0.95384(3) 0.073582(17) 0.01689(12) Uani 1 1 d .
Mo4 Mo 0.02279(3) 0.91605(3) -0.076455(15) 0.01421(11) Uani 1 1 d .
O1 O -0.1675(2) 0.8680(3) -0.06760(14) 0.0185(5) Uani 1 1 d .
O2 O -0.0535(2) 1.0891(3) -0.05154(13) 0.0158(5) Uani 1 1 d .
O3 O 0.2378(2) 0.7645(3) 0.05412(14) 0.0193(6) Uani 1 1 d .
O4 O 0.0276(2) 0.7312(3) -0.05629(13) 0.0174(5) Uani 1 1 d .
O5 O -0.0025(3) 0.9270(3) -0.16401(14) 0.0263(6) Uani 1 1 d .
O6 O -0.0969(2) 0.6820(3) 0.03947(13) 0.0179(6) Uani 1 1 d .
O7 O 0.0883(3) 0.6974(3) 0.15229(15) 0.0276(7) Uani 1 1 d .
O8 O 0.1162(3) 0.5223(3) 0.04800(14) 0.0208(6) Uani 1 1 d .
O9 O 0.1785(2) 0.9712(3) -0.04878(14) 0.0218(6) Uani 1 1 d .
O10 O 0.2902(3) 0.9491(3) 0.16192(15) 0.0277(7) Uani 1 1 d .
O11 O -0.1873(3) 0.6435(3) -0.15839(15) 0.0315(7) Uani 1 1 d .
O12 O 0.3957(3) 1.0014(3) 0.05182(17) 0.0306(7) Uani 1 1 d .
O13 O -0.3253(3) 0.6480(3) -0.05889(17) 0.0312(7) Uani 1 1 d .
N2 N -0.2028(3) 0.0353(4) -0.40096(18) 0.0276(8) Uani 1 1 d .
H2 H -0.1731 -0.0345 -0.4211 0.033 Uiso 1 1 calc R
N1 N -0.7227(4) 0.1788(4) -0.1159(2) 0.0344(9) Uani 1 1 d .
H1 H -0.7692 0.1240 -0.0960 0.041 Uiso 1 1 calc R
C1 C -0.5771(4) 0.3435(4) -0.1787(2) 0.0229(8) Uani 1 1 d .
C17 C -0.1423(4) 0.0764(5) -0.3390(2) 0.0305(10) Uani 1 1 d .
H17A H -0.0674 0.0313 -0.3171 0.037 Uiso 1 1 calc R
C18 C -0.6069(5) 0.2070(5) -0.0818(2) 0.0349(11) Uani 1 1 d .
H18A H -0.5762 0.1691 -0.0370 0.042 Uiso 1 1 calc R
C19 C -0.5321(4) 0.2914(5) -0.1121(2) 0.0292(10) Uani 1 1 d .
H19A H -0.4502 0.3140 -0.0878 0.035 Uiso 1 1 calc R
C2 C -0.1874(5) 0.1842(5) -0.3060(2) 0.0358(11) Uani 1 1 d .
H2A H -0.1447 0.2122 -0.2611 0.043 Uiso 1 1 calc R
C21 C -0.6989(4) 0.3139(5) -0.2115(2) 0.0279(9) Uani 1 1 d .
H21A H -0.7324 0.3509 -0.2562 0.034 Uiso 1 1 calc R
C22 C -0.3069(5) 0.0961(5) -0.4337(2) 0.0342(11) Uani 1 1 d .
H22A H -0.3477 0.0645 -0.4784 0.041 Uiso 1 1 calc R
C23 C -0.4906(4) 0.4180(4) -0.2168(2) 0.0258(9) Uani 1 1 d .
H23A H -0.4218 0.4623 -0.1834 0.031 Uiso 1 1 calc R
H23B H -0.5368 0.4899 -0.2475 0.031 Uiso 1 1 calc R
C24 C -0.2948(4) 0.2515(5) -0.3385(2) 0.0305(10) Uani 1 1 d .
C25 C -0.4385(4) 0.3092(4) -0.2604(3) 0.0325(10) Uani 1 1 d .
H25A H -0.3956 0.2368 -0.2288 0.039 Uiso 1 1 calc R
H25B H -0.5091 0.2654 -0.2927 0.039 Uiso 1 1 calc R
C26 C -0.3558(5) 0.2041(5) -0.4034(2) 0.0371(11) Uani 1 1 d .
H26A H -0.4312 0.2465 -0.4266 0.045 Uiso 1 1 calc R
C27 C -0.3475(5) 0.3668(5) -0.3021(2) 0.0353(11) Uani 1 1 d .
H27A H -0.3912 0.4334 -0.3369 0.042 Uiso 1 1 calc R
H27B H -0.2788 0.4156 -0.2707 0.042 Uiso 1 1 calc R
C28 C -0.7715(5) 0.2301(5) -0.1789(2) 0.0358(11) Uani 1 1 d .
H28A H -0.8552 0.2092 -0.2009 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
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O7 Mo1 O8 102.96(14) . .
O7 Mo1 O6 99.92(14) . .
O8 Mo1 O6 100.07(12) . .
O7 Mo1 O3 101.57(14) . .
O8 Mo1 O3 90.60(12) . .
O6 Mo1 O3 153.16(11) . .
O7 Mo1 O2 96.09(13) . 3_575
O8 Mo1 O2 157.44(12) . 3_575
O6 Mo1 O2 88.29(11) . 3_575
O3 Mo1 O2 73.65(10) . 3_575
O7 Mo1 O4 169.20(13) . .
O8 Mo1 O4 87.43(11) . .
O6 Mo1 O4 75.03(10) . .
O3 Mo1 O4 80.99(11) . .
O2 Mo1 O4 74.44(10) 3_575 .
O7 Mo1 Mo3 90.39(11) . .
O8 Mo1 Mo3 123.28(9) . .
O6 Mo1 Mo3 131.89(8) . .
O3 Mo1 Mo3 32.80(8) . .
O2 Mo1 Mo3 43.73(7) 3_575 .
O4 Mo1 Mo3 86.24(7) . .
O11 Mo2 O13 105.53(16) . .
O11 Mo2 O1 99.97(13) . .
O13 Mo2 O1 98.63(13) . .
O11 Mo2 O8 93.37(13) . 3_565
O13 Mo2 O8 98.34(13) . 3_565
O1 Mo2 O8 154.71(11) . 3_565
O11 Mo2 O6 160.13(13) . .
O13 Mo2 O6 93.20(13) . .
O1 Mo2 O6 83.38(11) . .
O8 Mo2 O6 77.09(10) 3_565 .
O11 Mo2 O4 91.88(13) . .
O13 Mo2 O4 161.37(13) . .
O1 Mo2 O4 71.30(10) . .
O8 Mo2 O4 86.98(10) 3_565 .
O6 Mo2 O4 70.49(9) . .
O10 Mo3 O12 104.93(16) . .
O10 Mo3 O3 99.86(13) . .
O12 Mo3 O3 106.82(14) . .
O10 Mo3 O1 94.53(13) . 3_575
O12 Mo3 O1 101.77(13) . 3_575
O3 Mo3 O1 143.23(11) . 3_575
O10 Mo3 O2 100.33(13) . 3_575
O12 Mo3 O2 154.33(13) . 3_575
O3 Mo3 O2 72.78(10) . 3_575
O1 Mo3 O2 71.42(10) 3_575 3_575
O10 Mo3 O9 170.15(12) . .
O12 Mo3 O9 83.59(13) . .
O3 Mo3 O9 82.01(11) . .
O1 Mo3 O9 78.67(10) 3_575 .
O2 Mo3 O9 70.86(9) 3_575 .
O10 Mo3 Mo1 91.44(11) . .
O12 Mo3 Mo1 141.17(11) . .
O3 Mo3 Mo1 34.74(8) . .
O1 Mo3 Mo1 111.92(8) 3_575 .
O2 Mo3 Mo1 40.92(7) 3_575 .
O9 Mo3 Mo1 84.63(7) . .
O5 Mo4 O9 103.98(15) . .
O5 Mo4 O4 105.82(13) . .
O9 Mo4 O4 104.37(12) . .
O5 Mo4 O2 102.01(13) . .
O9 Mo4 O2 95.39(12) . .
O4 Mo4 O2 140.45(11) . .
O5 Mo4 O1 97.77(13) . .
O9 Mo4 O1 157.10(11) . .
O4 Mo4 O1 75.99(11) . .
O2 Mo4 O1 72.86(10) . .
O5 Mo4 O2 177.05(12) . 3_575
O9 Mo4 O2 76.74(11) . 3_575
O4 Mo4 O2 76.64(10) . 3_575
O2 Mo4 O2 75.05(11) . 3_575
O1 Mo4 O2 81.18(10) . 3_575
Mo2 O1 Mo3 147.59(15) . 3_575
Mo2 O1 Mo4 104.84(11) . .
Mo3 O1 Mo4 106.45(12) 3_575 .
Mo4 O2 Mo1 147.46(14) . 3_575
Mo4 O2 Mo3 104.44(11) . 3_575
Mo1 O2 Mo3 95.35(10) 3_575 3_575
Mo4 O2 Mo4 104.95(11) . 3_575
Mo1 O2 Mo4 97.99(10) 3_575 3_575
Mo3 O2 Mo4 96.61(10) 3_575 3_575
Mo3 O3 Mo1 112.46(13) . .
Mo4 O4 Mo2 104.63(12) . .
Mo4 O4 Mo1 110.60(12) . .
Mo2 O4 Mo1 95.17(10) . .
Mo1 O6 Mo2 117.38(13) . .
Mo1 O8 Mo2 155.99(16) . 3_565
Mo4 O9 Mo3 114.87(13) . .
C17 N2 C22 121.9(4) . .
C17 N2 H2 119.0 . .
C22 N2 H2 119.0 . .
C18 N1 C28 122.9(4) . .
C18 N1 H1 118.6 . .
C28 N1 H1 118.5 . .
C21 C1 C19 118.7(4) . .
C21 C1 C23 120.7(4) . .
C19 C1 C23 120.3(4) . .
N2 C17 C2 120.3(4) . .
N2 C17 H17A 119.9 . .
C2 C17 H17A 119.9 . .
N1 C18 C19 119.6(4) . .
N1 C18 H18A 120.2 . .
C19 C18 H18A 120.2 . .
C18 C19 C1 119.7(4) . .
C18 C19 H19A 120.2 . .
C1 C19 H19A 120.2 . .
C17 C2 C24 119.8(4) . .
C17 C2 H2A 120.1 . .
C24 C2 H2A 120.1 . .
C28 C21 C1 119.7(4) . .
C28 C21 H21A 120.1 . .
C1 C21 H21A 120.1 . .
N2 C22 C26 120.3(4) . .
N2 C22 H22A 119.8 . .
C26 C22 H22A 119.8 . .
C1 C23 C25 106.7(3) . .
C1 C23 H23A 110.4 . .
C25 C23 H23A 110.4 . .
C1 C23 H23B 110.4 . .
C25 C23 H23B 110.4 . .
H23A C23 H23B 108.6 . .
C2 C24 C26 117.9(4) . .
C2 C24 C27 120.4(4) . .
C26 C24 C27 121.6(4) . .
C27 C25 C23 113.8(4) . .
C27 C25 H25A 108.8 . .
C23 C25 H25A 108.8 . .
C27 C25 H25B 108.8 . .
C23 C25 H25B 108.8 . .
H25A C25 H25B 107.7 . .
C22 C26 C24 119.7(5) . .
C22 C26 H26A 120.1 . .
C24 C26 H26A 120.1 . .
C24 C27 C25 109.7(4) . .
C24 C27 H27A 109.7 . .
C25 C27 H27A 109.7 . .
C24 C27 H27B 109.7 . .
C25 C27 H27B 109.7 . .
H27A C27 H27B 108.2 . .
N1 C28 C21 119.3(4) . .
N1 C28 H28A 120.3 . .
C21 C28 H28A 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O7 1.682(3) .
Mo1 O8 1.803(3) .
Mo1 O6 1.818(3) .
Mo1 O3 1.983(3) .
Mo1 O2 2.116(3) 3_575
Mo1 O4 2.361(3) .
Mo1 Mo3 3.2156(6) .
Mo2 O11 1.694(3) .
Mo2 O13 1.699(3) .
Mo2 O1 1.953(3) .
Mo2 O8 1.986(3) 3_565
Mo2 O6 2.189(3) .
Mo2 O4 2.282(3) .
Mo3 O10 1.698(3) .
Mo3 O12 1.705(3) .
Mo3 O3 1.885(3) .
Mo3 O1 1.989(3) 3_575
Mo3 O2 2.232(3) 3_575
Mo3 O9 2.388(3) .
Mo4 O5 1.688(3) .
Mo4 O9 1.760(3) .
Mo4 O4 1.839(3) .
Mo4 O2 1.983(3) .
Mo4 O1 2.172(3) .
Mo4 O2 2.467(3) 3_575
O1 Mo3 1.989(3) 3_575
O2 Mo1 2.116(3) 3_575
O2 Mo3 2.232(3) 3_575
O2 Mo4 2.467(3) 3_575
O8 Mo2 1.986(3) 3_565
N2 C17 1.322(6) .
N2 C22 1.325(6) .
N2 H2 0.8800 .
N1 C18 1.333(7) .
N1 C28 1.339(6) .
N1 H1 0.8800 .
C1 C21 1.385(6) .
C1 C19 1.394(6) .
C1 C23 1.506(5) .
C17 C2 1.374(7) .
C17 H17A 0.9500 .
C18 C19 1.376(7) .
C18 H18A 0.9500 .
C19 H19A 0.9500 .
C2 C24 1.381(7) .
C2 H2A 0.9500 .
C21 C28 1.382(6) .
C21 H21A 0.9500 .
C22 C26 1.369(7) .
C22 H22A 0.9500 .
C23 C25 1.541(6) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 C26 1.390(6) .
C24 C27 1.505(6) .
C25 C27 1.519(6) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 H26A 0.9500 .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C28 H28A 0.9500 .
