#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:37:41 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223563 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/42/7234235.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_7234235
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            'C21 H22 Cd Mo4 N9 O18'
_chemical_formula_weight         1184.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                117.2860(10)
_cell_angle_beta                 101.6580(10)
_cell_angle_gamma                104.9900(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2427(5)
_cell_length_b                   12.7055(5)
_cell_length_c                   12.9947(5)
_cell_measurement_reflns_used    4716
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.426
_cell_measurement_theta_min      1.856
_cell_volume                     1609.70(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0173
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.426
_diffrn_reflns_theta_min         1.856
_exptl_absorpt_coefficient_mu    2.261
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    2.444
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1142
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_transmission_factor_max   0.789
_exptl_transmission_factor_min   0.728
_refine_diff_density_max         1.985
_refine_diff_density_min         -3.684
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0335
_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)+(0.0211P)²+4.7524P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6530
_reflns_number_total             8031
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce01394f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7234233--7234237.cif.'
_cod_original_cell_volume        1609.69(11)
_cod_database_code               7234235
_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   0.728
_shelx_estimated_absorpt_t_max   0.789
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cd1 Cd 0.14299(3) 0.34999(3) 0.73274(3) 0.02666(8) Uani 1 1 d . .
Mo1 Mo 0.24981(3) 0.71140(3) 0.83785(3) 0.02221(8) Uani 1 1 d . .
O1 O 0.3217(2) 0.3319(3) 0.7128(3) 0.0283(6) Uani 1 1 d . .
C1 C 0.1468(4) 0.3694(5) 0.3985(5) 0.0426(12) Uani 1 1 d . .
H1A H 0.1190 0.3784 0.3295 0.051 Uiso 1 1 d R U
N1 N 0.1501(3) 0.3468(4) 0.5573(3) 0.0261(7) Uani 1 1 d . .
O1W O 1.4767(3) 0.4011(4) 1.0201(3) 0.0453(9) Uani 1 1 d . .
H1WB H 1.4954 0.3444 1.0276 0.054 Uiso 1 1 d R U
Mo2 Mo 0.49837(3) 0.74072(3) 0.76815(3) 0.02267(8) Uani 1 1 d . .
O2 O 0.9947(3) 0.3935(3) 0.7968(3) 0.0315(7) Uani 1 1 d . .
C2 C 0.2545(4) 0.3601(5) 0.4372(5) 0.0375(11) Uani 1 1 d . .
H2A H 0.3179 0.3639 0.4042 0.045 Uiso 1 1 d R U
N2 N 0.0872(3) 0.3614(4) 0.4716(4) 0.0342(9) Uani 1 1 d . .
H2B H 0.0171 0.3652 0.4646 0.041 Uiso 1 1 calc R U
O2W O -0.1401(3) 0.3318(4) 0.4863(3) 0.0462(9) Uani 1 1 d . .
H2WB H -0.1918 0.3150 0.4205 0.055 Uiso 1 1 d R U
Mo3 Mo 0.75852(3) 1.02540(4) 0.94171(4) 0.02715(9) Uani 1 1 d . .
C3 C 0.2529(3) 0.3457(4) 0.5374(4) 0.0221(8) Uani 1 1 d . .
O3 O -0.1454(3) 0.1402(4) 0.5338(4) 0.0452(9) Uani 1 1 d . .
N3 N 0.4383(3) 0.3215(3) 0.5955(3) 0.0225(7) Uani 1 1 d . .
H3A H 0.4370 0.3078 0.5208 0.027 Uiso 1 1 d R U
Mo4 Mo 0.42874(3) 1.04645(4) 0.90270(4) 0.03495(10) Uani 1 1 d . .
O4 O 0.2511(3) 0.5757(3) 0.8363(3) 0.0326(7) Uani 1 1 d . .
N4 N 0.8612(3) 0.3371(3) 0.8787(3) 0.0227(7) Uani 1 1 d . .
H4A H 0.8526 0.3183 0.9363 0.027 Uiso 1 1 d R U
C4 C 0.3406(3) 0.3318(4) 0.6218(4) 0.0217(8) Uani 1 1 d . .
N5 N 1.1684(3) 0.3631(3) 0.9272(3) 0.0266(7) Uani 1 1 d . .
C5 C 0.5441(3) 0.3279(4) 0.6721(4) 0.0204(8) Uani 1 1 d . .
O5 O 0.4961(3) 0.6021(3) 0.7549(3) 0.0417(8) Uani 1 1 d . .
C6 C 0.5439(4) 0.2949(5) 0.7592(4) 0.0311(10) Uani 1 1 d . .
H6A H 0.4701 0.2670 0.7721 0.037 Uiso 1 1 d R U
N6 N 1.2360(3) 0.3394(4) 1.0023(3) 0.0331(8) Uani 1 1 d . .
H6B H 1.3088 0.3448 1.0085 0.040 Uiso 1 1 calc R U
O6 O 0.6572(3) 0.8561(3) 0.8992(4) 0.0500(10) Uani 1 1 d . .
C7 C 0.6507(4) 0.3017(5) 0.8272(4) 0.0320(10) Uani 1 1 d . .
H7A H 0.6508 0.2797 0.8887 0.038 Uiso 1 1 d R U
N7 N 0.0613(3) 0.1304(4) 0.6582(4) 0.0313(8) Uani 1 1 d . .
O7 O 0.7593(3) 0.9881(3) 0.7992(3) 0.0440(8) Uani 1 1 d . .
O8 O 0.5221(3) 0.7302(4) 0.6402(3) 0.0482(9) Uani 1 1 d . .
C8 C 0.7579(3) 0.3397(4) 0.8089(4) 0.0211(8) Uani 1 1 d . .
N8 N 0.1345(3) 0.0885(4) 0.7061(4) 0.0362(9) Uani 1 1 d . .
H8A H 0.2123 0.1191 0.7267 0.043 Uiso 1 1 calc R U
O9 O 0.5163(3) 0.9616(3) 0.8400(3) 0.0459(9) Uani 1 1 d . .
C9 C 0.7577(4) 0.3750(5) 0.7218(4) 0.0300(9) Uani 1 1 d . .
H9B H 0.8313 0.4032 0.7085 0.036 Uiso 1 1 d R U
N9 N -0.2607(3) 0.0236(4) 0.5937(4) 0.0325(8) Uani 1 1 d . .
H9A H -0.2538 -0.0146 0.6370 0.039 Uiso 1 1 d R U
C10 C 0.6510(4) 0.3688(5) 0.6548(4) 0.0313(10) Uani 1 1 d . .
H10A H 0.6504 0.3935 0.5951 0.038 Uiso 1 1 d R U
O10 O 0.8974(3) 1.0518(3) 1.0253(3) 0.0385(8) Uani 1 1 d . .
C11 C 0.9698(3) 0.3598(4) 0.8686(4) 0.0225(8) Uani 1 1 d . .
O11 O 0.5387(3) 1.1914(3) 1.0473(3) 0.0274(6) Uani 1 1 d . .
C12 C 1.0629(3) 0.3425(4) 0.9445(4) 0.0216(8) Uani 1 1 d . .
O12 O 0.3669(3) 1.0900(3) 0.8077(3) 0.0428(9) Uani 1 1 d . .
C13 C 1.0634(4) 0.3075(5) 1.0312(4) 0.0333(10) Uani 1 1 d . .
H13A H 0.9999 0.2897 1.0613 0.040 Uiso 1 1 d R U
O13 O 0.3310(2) 0.7127(3) 0.7250(3) 0.0267(6) Uani 1 1 d . .
C14 C 1.1779(4) 0.3068(5) 1.0659(5) 0.0383(11) Uani 1 1 d . .
H14A H 1.2089 0.2860 1.1249 0.046 Uiso 1 1 d R U
O14 O 0.3052(3) 0.9256(3) 0.8986(3) 0.0304(7) Uani 1 1 d . .
C15 C 0.0737(5) -0.0055(5) 0.7184(5) 0.0428(12) Uani 1 1 d . .
H15A H 0.1080 -0.0506 0.7484 0.051 Uiso 1 1 d R U
O15 O 0.1072(3) 0.6647(4) 0.7432(3) 0.0422(8) Uani 1 1 d . .
C16 C -0.0464(4) -0.0270(5) 0.6783(5) 0.0393(11) Uani 1 1 d . .
H16A H -0.1136 -0.0887 0.6755 0.047 Uiso 1 1 d R U
O16 O 0.7601(3) 1.1955(3) 1.0011(3) 0.0287(6) Uani 1 1 d . .
C17 C -0.0509(4) 0.0598(4) 0.6410(4) 0.0288(9) Uani 1 1 d . .
C18 C -0.1563(4) 0.0800(4) 0.5851(4) 0.0282(9) Uani 1 1 d . .
C19 C -0.3798(4) 0.0152(4) 0.5456(4) 0.0278(9) Uani 1 1 d . .
C20 C -0.4149(4) 0.0444(5) 0.4574(4) 0.0358(10) Uani 1 1 d . .
H20A H -0.3570 0.0753 0.4271 0.043 Uiso 1 1 d R U
C21 C -0.5353(4) 0.0287(5) 0.4128(4) 0.0362(11) Uani 1 1 d . .
H21A H -0.5460 0.0527 0.3526 0.054 Uiso 1 1 d R U
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
O2 Cd1 N1 117.63(11) 1_455 .
O2 Cd1 O1 167.43(11) 1_455 .
N1 Cd1 O1 72.50(11) . .
O2 Cd1 N7 96.37(12) 1_455 .
N1 Cd1 N7 101.89(13) . .
O1 Cd1 N7 88.24(12) . .
O2 Cd1 O4 86.80(11) 1_455 .
N1 Cd1 O4 84.77(12) . .
O1 Cd1 O4 86.82(11) . .
N7 Cd1 O4 170.12(12) . .
O2 Cd1 N5 70.06(11) 1_455 1_455
N1 Cd1 N5 171.30(11) . 1_455
O1 Cd1 N5 99.34(10) . 1_455
N7 Cd1 N5 80.49(13) . 1_455
O4 Cd1 N5 91.87(11) . 1_455
O15 Mo1 O4 104.73(17) . .
O15 Mo1 O16 100.71(15) . 2_677
O4 Mo1 O16 98.46(13) . 2_677
O15 Mo1 O13 97.82(14) . .
O4 Mo1 O13 101.94(14) . .
O16 Mo1 O13 147.85(13) 2_677 .
O15 Mo1 O14 93.56(15) . .
O4 Mo1 O14 160.87(13) . .
O16 Mo1 O14 72.19(11) 2_677 .
O13 Mo1 O14 80.67(11) . .
O15 Mo1 O11 166.56(14) . 2_677
O4 Mo1 O11 86.76(13) . 2_677
O16 Mo1 O11 84.14(11) 2_677 2_677
O13 Mo1 O11 72.58(11) . 2_677
O14 Mo1 O11 75.87(10) . 2_677
C4 O1 Cd1 115.4(2) . .
N2 C1 C2 108.0(4) . .
C3 N1 N2 106.0(3) . .
C3 N1 Cd1 114.7(3) . .
N2 N1 Cd1 138.7(3) . .
O5 Mo2 O8 104.40(18) . .
O5 Mo2 O13 102.83(15) . .
O8 Mo2 O13 101.09(14) . .
O5 Mo2 O6 98.25(15) . .
O8 Mo2 O6 102.88(17) . .
O13 Mo2 O6 142.81(15) . .
O5 Mo2 O11 91.69(14) . 2_677
O8 Mo2 O11 163.86(15) . 2_677
O13 Mo2 O11 73.66(11) . 2_677
O6 Mo2 O11 75.45(14) . 2_677
O5 Mo2 O9 166.44(15) . .
O8 Mo2 O9 87.93(16) . .
O13 Mo2 O9 79.84(12) . .
O6 Mo2 O9 73.09(13) . .
O11 Mo2 O9 76.19(12) 2_677 .
C11 O2 Cd1 116.7(3) . 1_655
C1 C2 C3 104.5(4) . .
C1 N2 N1 111.4(4) . .
O10 Mo3 O7 106.21(17) . .
O10 Mo3 O16 104.71(15) . .
O7 Mo3 O16 97.90(15) . .
O10 Mo3 O6 103.60(15) . .
O7 Mo3 O6 99.26(18) . .
O16 Mo3 O6 141.06(15) . .
O10 Mo3 O14 93.72(14) . 2_677
O7 Mo3 O14 159.88(14) . 2_677
O16 Mo3 O14 73.81(11) . 2_677
O6 Mo3 O14 78.21(15) . 2_677
N1 C3 C2 110.1(4) . .
N1 C3 C4 117.0(3) . .
C2 C3 C4 132.8(4) . .
C4 N3 C5 126.9(3) . .
O12 Mo4 O9 110.05(17) . .
O12 Mo4 O11 108.36(15) . .
O9 Mo4 O11 104.13(14) . .
O12 Mo4 O14 108.18(14) . .
O9 Mo4 O14 103.53(14) . .
O11 Mo4 O14 122.09(13) . .
Mo1 O4 Cd1 143.98(17) . .
C11 N4 C8 127.0(3) . .
O1 C4 N3 123.6(4) . .
O1 C4 C3 120.1(3) . .
N3 C4 C3 116.3(3) . .
C12 N5 N6 104.6(3) . .
C12 N5 Cd1 110.6(3) . 1_655
N6 N5 Cd1 139.5(3) . 1_655
C6 C5 C10 119.9(4) . .
C6 C5 N3 123.7(3) . .
C10 C5 N3 116.5(3) . .
C5 C6 C7 119.4(4) . .
C14 N6 N5 112.4(4) . .
Mo3 O6 Mo2 127.35(17) . .
C6 C7 C8 121.4(4) . .
C17 N7 N8 104.8(4) . .
C17 N7 Cd1 127.0(3) . .
N8 N7 Cd1 115.8(3) . .
C7 C8 C9 118.9(4) . .
C7 C8 N4 117.2(3) . .
C9 C8 N4 124.0(3) . .
C15 N8 N7 112.7(4) . .
Mo4 O9 Mo2 132.54(18) . .
C10 C9 C8 119.4(4) . .
C18 N9 C19 130.2(4) . .
C9 C10 C5 121.1(4) . .
O2 C11 N4 122.3(4) . .
O2 C11 C12 119.5(3) . .
N4 C11 C12 118.2(3) . .
Mo4 O11 Mo2 120.73(13) . 2_677
Mo4 O11 Mo1 138.56(15) . 2_677
Mo2 O11 Mo1 90.31(10) 2_677 2_677
N5 C12 C13 111.8(4) . .
N5 C12 C11 115.2(3) . .
C13 C12 C11 133.0(4) . .
C12 C13 C14 103.8(4) . .
Mo2 O13 Mo1 120.21(14) . .
N6 C14 C13 107.4(4) . .
Mo4 O14 Mo3 121.63(16) . 2_677
Mo4 O14 Mo1 136.07(15) . .
Mo3 O14 Mo1 92.98(11) 2_677 .
N8 C15 C16 107.1(4) . .
C15 C16 C17 105.2(4) . .
Mo1 O16 Mo3 118.20(14) 2_677 .
N7 C17 C16 110.3(4) . .
N7 C17 C18 118.8(4) . .
C16 C17 C18 130.9(4) . .
O3 C18 N9 125.2(4) . .
O3 C18 C17 120.8(4) . .
N9 C18 C17 114.0(4) . .
C21 C19 C20 119.0(4) 2_456 .
C21 C19 N9 117.2(4) 2_456 .
C20 C19 N9 123.7(4) . .
C19 C20 C21 119.4(4) . .
C19 C21 C20 121.7(4) 2_456 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O2 2.237(3) 1_455
Cd1 N1 2.282(3) .
Cd1 O1 2.312(3) .
Cd1 N7 2.326(4) .
Cd1 O4 2.359(3) .
Cd1 N5 2.404(3) 1_455
Mo1 O15 1.686(3) .
Mo1 O4 1.720(3) .
Mo1 O16 1.924(3) 2_677
Mo1 O13 1.934(3) .
Mo1 O14 2.312(3) .
Mo1 O11 2.356(3) 2_677
O1 C4 1.250(5) .
C1 N2 1.334(6) .
C1 C2 1.369(6) .
N1 C3 1.337(5) .
N1 N2 1.335(5) .
Mo2 O5 1.682(3) .
Mo2 O8 1.696(3) .
Mo2 O13 1.901(3) .
Mo2 O6 1.931(3) .
Mo2 O11 2.334(3) 2_677
Mo2 O9 2.448(3) .
O2 C11 1.248(5) .
O2 Cd1 2.237(3) 1_655
C2 C3 1.399(6) .
Mo3 O10 1.676(3) .
Mo3 O7 1.691(3) .
Mo3 O16 1.926(3) .
Mo3 O6 1.930(3) .
Mo3 O14 2.241(3) 2_677
C3 C4 1.479(5) .
O3 C18 1.223(5) .
N3 C4 1.330(5) .
N3 C5 1.424(5) .
Mo4 O12 1.695(3) .
Mo4 O9 1.766(4) .
Mo4 O11 1.805(3) .
Mo4 O14 1.827(3) .
N4 C11 1.333(5) .
N4 C8 1.418(5) .
N5 C12 1.336(5) .
N5 N6 1.341(5) .
N5 Cd1 2.404(3) 1_655
C5 C6 1.374(5) .
C5 C10 1.382(5) .
C6 C7 1.380(6) .
N6 C14 1.327(6) .
C7 C8 1.384(5) .
N7 C17 1.340(5) .
N7 N8 1.341(5) .
C8 C9 1.395(5) .
N8 C15 1.329(6) .
C9 C10 1.377(6) .
N9 C18 1.348(5) .
N9 C19 1.421(5) .
C11 C12 1.482(5) .
O11 Mo2 2.334(3) 2_677
O11 Mo1 2.356(3) 2_677
C12 C13 1.387(6) .
C13 C14 1.387(6) .
O14 Mo3 2.242(3) 2_677
C15 C16 1.364(7) .
C16 C17 1.400(6) .
O16 Mo1 1.924(3) 2_677
C17 C18 1.492(6) .
C19 C21 1.374(6) 2_456
C19 C20 1.382(6) .
C20 C21 1.394(6) .
C21 C19 1.374(6) 2_456
