#------------------------------------------------------------------------------
#$Date: 2019-11-07 20:37:41 +0100 (jue 07 de nov de 2019) $
#$Revision: 223563 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/42/7234237.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_7234237
loop_
_publ_author_name
'Pan, Xiang'
'Wang, Xiuli'
'Wang, Xiang'
'Li, Yan'
'Liu, Guocheng'
'Lin, Hongyan'
_publ_section_title
;
 Various types of isopolymolybdate-based metal--organic complexes formed
 in different conditions: synthesis, structures, luminescence,
 electrochemical, and photocatalytic performances
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6472
_journal_paper_doi               10.1039/C9CE01394F
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C10 H14 Mo3 N6 O13 Zn'
_chemical_formula_weight         779.46
_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   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-13 deposited with the CCDC.    2019-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.9260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9855(5)
_cell_length_b                   19.6775(7)
_cell_length_c                   7.6312(3)
_cell_measurement_reflns_used    6397
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.263
_cell_measurement_theta_min      1.609
_cell_volume                     1900.53(12)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'sealed tube'
_diffrn_measurement_method       graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13794
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.263
_diffrn_reflns_theta_min         1.609
_exptl_absorpt_coefficient_mu    3.267
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    2.724
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_transmission_factor_max   0.715
_exptl_transmission_factor_min   0.640
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0228
_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)+(0.0306P)²+2.6599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4069
_reflns_number_total             4701
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce01394f2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7234233--7234237.cif.'
_cod_database_code               7234237
_shelx_shelxl_version_number     2014/7
_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   0.640
_shelx_estimated_absorpt_t_max   0.715
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_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mo1 Mo -0.02926(2) 0.35276(2) 0.02688(3) 0.01271(6) Uani 1 1 d . .
Zn1 Zn 0.28352(3) 0.36700(2) -0.37617(5) 0.02243(9) Uani 1 1 d . .
O1 O 0.19031(16) 0.32047(10) -0.1863(3) 0.0195(4) Uani 1 1 d . .
C1 C 0.3760(3) 0.21983(17) -0.3201(5) 0.0308(7) Uani 1 1 d . .
H1A H 0.3154 0.1952 -0.3844 0.037 Uiso 1 1 d R U
O1W O 0.5745(4) 0.0817(2) -0.0580(6) 0.1148(19) Uani 1 1 d . .
H1WA H 0.5934 0.0731 -0.1553 0.138 Uiso 1 1 d R U
H1WB H 0.6257 0.1017 0.0121 0.138 Uiso 1 1 d R U
N1 N 0.1925(2) 0.45203(12) -0.3876(3) 0.0208(5) Uani 1 1 d . .
Mo2 Mo -0.17276(2) 0.25174(2) 0.22949(3) 0.01214(6) Uani 1 1 d . .
O2 O 0.33304(18) 0.41971(11) -0.5874(3) 0.0254(5) Uani 1 1 d . .
N2 N 0.3837(2) 0.28706(14) -0.3102(3) 0.0235(5) Uani 1 1 d . .
C2 C 0.4822(2) 0.30070(17) -0.2041(4) 0.0255(7) Uani 1 1 d . .
Mo3 Mo 0.10609(2) 0.25326(2) -0.18281(3) 0.01026(6) Uani 1 1 d . .
O3 O 0.43010(19) 0.41335(13) -0.1945(3) 0.0348(6) Uani 1 1 d . .
C3 C 0.5332(3) 0.24121(18) -0.1513(5) 0.0332(8) Uani 1 1 d . .
H3A H 0.6028 0.2357 -0.0769 0.040 Uiso 1 1 d R U
N3 N 0.7160(2) 0.49339(14) -0.2203(4) 0.0274(6) Uani 1 1 d . .
H3B H 0.7504 0.4534 -0.2016 0.033 Uiso 1 1 d R U
O4 O -0.02837(15) 0.31481(10) -0.2106(2) 0.0136(4) Uani 1 1 d . .
C4 C 0.5041(2) 0.37174(16) -0.1566(4) 0.0236(6) Uani 1 1 d . .
N4 N 0.0984(2) 0.54448(14) -0.3867(4) 0.0299(6) Uani 1 1 d . .
H4A H 0.0550 0.5750 -0.3529 0.036 Uiso 1 1 d R U
O5 O 0.08167(15) 0.26645(10) 0.0691(2) 0.0144(4) Uani 1 1 d . .
N5 N 0.4652(2) 0.19144(15) -0.2261(4) 0.0366(7) Uani 1 1 d . .
H5B H 0.4783 0.1466 -0.2148 0.044 Uiso 1 1 d R U
C5 C 0.1437(3) 0.55062(16) -0.5298(4) 0.0272(7) Uani 1 1 d . .
H5A H 0.1365 0.5879 -0.6129 0.033 Uiso 1 1 d R U
O6 O 0.07455(19) 0.40789(11) 0.0643(3) 0.0295(5) Uani 1 1 d . .
C6 C 0.6302(3) 0.45401(16) 0.0161(4) 0.0258(7) Uani 1 1 d . .
H6A H 0.6970 0.4494 0.0999 0.031 Uiso 1 1 d R U
H6B H 0.5786 0.4664 0.0829 0.031 Uiso 1 1 d R U
N6 N 0.6013(2) 0.38842(14) -0.0690(4) 0.0294(6) Uani 1 1 d . .
H6C H 0.6524 0.3571 -0.0632 0.035 Uiso 1 1 d R U
O7 O -0.13879(19) 0.40394(11) -0.0239(3) 0.0271(5) Uani 1 1 d . .
C7 C 0.6398(3) 0.51056(17) -0.1145(5) 0.0280(7) Uani 1 1 d . .
H7A H 0.5720 0.5179 -0.1935 0.034 Uiso 1 1 d R U
H7B H 0.6609 0.5519 -0.0497 0.034 Uiso 1 1 d R U
O8 O -0.03079(15) 0.32044(10) 0.2645(2) 0.0138(4) Uani 1 1 d . .
C8 C 0.2763(2) 0.47049(15) -0.6381(4) 0.0221(6) Uani 1 1 d . .
O9 O -0.25447(17) 0.31970(12) 0.2247(3) 0.0251(5) Uani 1 1 d . .
C9 C 0.1293(3) 0.48470(17) -0.3024(4) 0.0262(7) Uani 1 1 d . .
H9A H 0.1083 0.4682 -0.1973 0.031 Uiso 1 1 d R U
O10 O -0.14063(16) 0.23838(10) 0.4879(2) 0.0155(4) Uani 1 1 d . .
C10 C 0.2012(2) 0.49302(15) -0.5317(4) 0.0204(6) Uani 1 1 d . .
O11 O -0.25690(17) 0.18487(11) 0.1641(3) 0.0244(5) Uani 1 1 d . .
O12 O 0.18944(16) 0.18806(10) -0.0904(2) 0.0184(4) Uani 1 1 d . .
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'
Zn Zn 0.2839 1.4301 '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
O6 Mo1 O7 104.43(12) . .
O6 Mo1 O8 103.12(9) . .
O7 Mo1 O8 102.94(9) . .
O6 Mo1 O4 103.24(9) . .
O7 Mo1 O4 100.99(9) . .
O8 Mo1 O4 138.34(8) . .
O6 Mo1 O5 89.97(10) . .
O7 Mo1 O5 165.39(10) . .
O8 Mo1 O5 75.64(7) . .
O4 Mo1 O5 72.72(7) . .
O6 Mo1 O10 167.71(10) . 4_565
O7 Mo1 O10 87.86(10) . 4_565
O8 Mo1 O10 73.94(7) . 4_565
O4 Mo1 O10 73.43(7) . 4_565
O5 Mo1 O10 77.74(7) . 4_565
N2 Zn1 N1 168.21(10) . .
N2 Zn1 O12 91.25(9) . 4_565
N1 Zn1 O12 99.13(9) . 4_565
N2 Zn1 O2 106.21(9) . .
N1 Zn1 O2 80.72(9) . .
O12 Zn1 O2 83.36(8) 4_565 .
N2 Zn1 O1 86.16(9) . .
N1 Zn1 O1 88.37(9) . .
O12 Zn1 O1 89.34(7) 4_565 .
O2 Zn1 O1 165.70(8) . .
N2 Zn1 O3 75.99(10) . .
N1 Zn1 O3 95.46(9) . .
O12 Zn1 O3 159.60(9) 4_565 .
O2 Zn1 O3 85.02(9) . .
O1 Zn1 O3 105.33(8) . .
Mo3 O1 Zn1 138.53(11) . .
N2 C1 N5 109.9(3) . .
C9 N1 C10 106.1(3) . .
C9 N1 Zn1 142.7(2) . .
C10 N1 Zn1 111.17(19) . .
O9 Mo2 O11 104.09(11) . .
O9 Mo2 O10 96.86(9) . .
O11 Mo2 O10 99.80(9) . .
O9 Mo2 O10 99.35(9) . 4_565
O11 Mo2 O10 93.30(9) . 4_565
O10 Mo2 O10 156.00(12) . 4_565
O9 Mo2 O4 161.66(9) . 4_566
O11 Mo2 O4 93.47(9) . 4_566
O10 Mo2 O4 74.60(7) . 4_566
O10 Mo2 O4 84.67(7) 4_565 4_566
O9 Mo2 O8 91.19(9) . .
O11 Mo2 O8 161.38(9) . .
O10 Mo2 O8 88.65(7) . .
O10 Mo2 O8 73.47(7) 4_565 .
O4 Mo2 O8 72.68(7) 4_566 .
C8 O2 Zn1 111.5(2) . .
C1 N2 C2 106.0(3) . .
C1 N2 Zn1 136.2(2) . .
C2 N2 Zn1 117.0(2) . .
C3 C2 N2 109.4(3) . .
C3 C2 C4 134.2(3) . .
N2 C2 C4 115.9(3) . .
O1 Mo3 O12 103.61(10) . .
O1 Mo3 O5 96.14(9) . 4_565
O12 Mo3 O5 101.91(9) . 4_565
O1 Mo3 O5 98.67(9) . .
O12 Mo3 O5 85.69(8) . .
O5 Mo3 O5 161.27(11) 4_565 .
O1 Mo3 O4 94.15(9) . .
O12 Mo3 O4 154.64(8) . .
O5 Mo3 O4 93.90(8) 4_565 .
O5 Mo3 O4 73.70(7) . .
O1 Mo3 O8 165.55(8) . 4_565
O12 Mo3 O8 89.54(8) . 4_565
O5 Mo3 O8 74.98(7) 4_565 4_565
O5 Mo3 O8 88.13(7) . 4_565
O4 Mo3 O8 75.43(7) . 4_565
C4 O3 Zn1 112.0(2) . .
N5 C3 C2 105.6(3) . .
C8 N3 C7 121.2(3) 3_664 .
Mo1 O4 Mo3 107.65(8) . .
Mo1 O4 Mo2 103.45(8) . 4_565
Mo3 O4 Mo2 108.78(8) . 4_565
O3 C4 N6 123.4(3) . .
O3 C4 C2 118.4(3) . .
N6 C4 C2 118.2(3) . .
C5 N4 C9 108.9(3) . .
Mo3 O5 Mo3 153.46(11) 4_566 .
Mo3 O5 Mo1 105.21(8) 4_566 .
Mo3 O5 Mo1 101.27(8) . .
C1 N5 C3 109.1(3) . .
N4 C5 C10 105.8(3) . .
N6 C6 C7 114.1(3) . .
C4 N6 C6 124.3(3) . .
N3 C7 C6 111.2(3) . .
Mo1 O8 Mo2 105.48(8) . .
Mo1 O8 Mo3 101.90(8) . 4_566
Mo2 O8 Mo3 103.08(8) . 4_566
O2 C8 N3 122.5(3) . 3_664
O2 C8 C10 119.2(3) . .
N3 C8 C10 118.2(3) 3_664 .
N1 C9 N4 109.8(3) . .
Mo2 O10 Mo2 152.50(11) . 4_566
Mo2 O10 Mo1 103.00(8) . 4_566
Mo2 O10 Mo1 102.37(8) 4_566 4_566
C5 C10 N1 109.5(3) . .
C5 C10 C8 133.7(3) . .
N1 C10 C8 116.4(3) . .
Mo3 O12 Zn1 154.32(11) . 4_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O6 1.704(2) .
Mo1 O7 1.715(2) .
Mo1 O8 1.9261(18) .
Mo1 O4 1.9625(18) .
Mo1 O5 2.2035(19) .
Mo1 O10 2.281(2) 4_565
Zn1 N2 2.031(3) .
Zn1 N1 2.039(3) .
Zn1 O12 2.1084(19) 4_565
Zn1 O2 2.133(2) .
Zn1 O1 2.277(2) .
Zn1 O3 2.279(2) .
O1 Mo3 1.720(2) .
C1 N2 1.328(4) .
C1 N5 1.341(4) .
N1 C9 1.322(4) .
N1 C10 1.389(4) .
Mo2 O9 1.702(2) .
Mo2 O11 1.712(2) .
Mo2 O10 1.9400(18) .
Mo2 O10 1.9888(18) 4_565
Mo2 O4 2.2485(19) 4_566
Mo2 O8 2.2533(19) .
O2 C8 1.251(4) .
N2 C2 1.379(4) .
C2 C3 1.361(5) .
C2 C4 1.456(4) .
Mo3 O12 1.7244(19) .
Mo3 O5 1.8890(18) 4_565
Mo3 O5 2.0334(18) .
Mo3 O4 2.0964(19) .
Mo3 O8 2.2593(19) 4_565
O3 C4 1.246(4) .
C3 N5 1.356(5) .
N3 C8 1.316(4) 3_664
N3 C7 1.450(4) .
O4 Mo2 2.2485(19) 4_565
C4 N6 1.331(4) .
N4 C5 1.356(4) .
N4 C9 1.358(4) .
O5 Mo3 1.8890(18) 4_566
C5 C10 1.360(4) .
C6 N6 1.456(4) .
C6 C7 1.517(4) .
O8 Mo3 2.2594(19) 4_566
C8 N3 1.316(4) 3_664
C8 C10 1.469(4) .
O10 Mo2 1.9887(18) 4_566
O10 Mo1 2.281(2) 4_566
O12 Zn1 2.1084(19) 4_566
