#------------------------------------------------------------------------------
#$Date: 2019-10-08 03:16:47 +0200 (mar 08 de oct de 2019) $
#$Revision: 219146 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/13/7701322.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_7701322
loop_
_publ_author_name
'Zhou, wanli'
'Liu, Ping'
'Zheng, yanping'
'Liu, Xuekun'
'Zhang, Yong'
'Yuan, Gang'
'Peng, Jun'
_publ_section_title
;
 Four new dual-functional electro-catalysts formed of small molybdenum
 clusters and Cu-pyridyl complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03560E
_journal_year                    2019
_chemical_formula_moiety         'C11 H11 Cu Mo3 N5 O11'
_chemical_formula_sum            'C11 H11 Cu Mo3 N5 O11'
_chemical_formula_weight         740.61
_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
;
2019-09-03 deposited with the CCDC.    2019-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                77.076(5)
_cell_angle_beta                 85.384(5)
_cell_angle_gamma                74.767(5)
_cell_formula_units_Z            2
_cell_length_a                   7.633(5)
_cell_length_b                   10.979(5)
_cell_length_c                   11.349(5)
_cell_measurement_reflns_used    12537
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.328
_cell_measurement_theta_min      2.963
_cell_volume                     894.2(8)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_data_reduction        CrysAlis
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12537
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.963
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.609
_exptl_transmission_factor_min   0.386
_refine_diff_density_max         1.178
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4425
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0241
_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)+(0.0252P)²+4.5487P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4239
_reflns_number_total             4425
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt03560e2.cif
_cod_data_source_block           3
_cod_database_code               7701322
_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.
;
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
Mo1 Mo 0.02807(3) 0.41708(2) 0.64996(2) 0.00548(6) Uani 1 1 d . .
Mo2 Mo -0.53186(3) 0.59889(2) 0.35272(2) 0.00749(6) Uani 1 1 d . .
Mo3 Mo -0.32118(3) 0.66069(2) 0.57118(2) 0.00949(6) Uani 1 1 d . .
Cu1 Cu -0.90225(5) 0.86828(4) 0.21053(4) 0.01466(9) Uani 1 1 d . .
O1 O -0.6298(3) 0.7627(2) 0.3117(2) 0.0190(5) Uani 1 1 d . .
O1W O -0.5734(5) 1.0245(3) 0.3148(3) 0.0354(7) Uani 1 1 d D .
H1WA H -0.524(8) 0.950(3) 0.357(5) 0.053 Uiso 1 1 d D U
H1WB H -0.577(8) 1.072(5) 0.365(4) 0.053 Uiso 1 1 d D U
O2 O 0.0259(3) 0.2533(2) 0.7013(2) 0.0164(5) Uani 1 1 d . .
O3 O -0.2424(3) 0.4487(2) 0.6277(2) 0.0129(4) Uani 1 1 d . .
O4 O -0.4531(3) 0.5556(3) 0.2192(2) 0.0197(5) Uani 1 1 d . .
O5 O 0.0208(3) 0.4701(2) 0.7804(2) 0.0187(5) Uani 1 1 d . .
O6 O -0.0574(3) 0.6031(2) 0.54697(19) 0.0108(4) Uani 1 1 d . .
O7 O -0.2763(3) 0.6007(2) 0.3891(2) 0.0131(4) Uani 1 1 d . .
O8 O -0.5307(3) 0.6044(2) 0.5449(2) 0.0116(4) Uani 1 1 d . .
O9 O -0.3400(3) 0.6727(3) 0.7191(2) 0.0208(5) Uani 1 1 d . .
O10 O -0.3684(3) 0.8194(2) 0.4932(2) 0.0222(5) Uani 1 1 d . .
C1 C -0.7473(5) 0.6745(4) 0.0363(3) 0.0230(7) Uani 1 1 d . .
H1A H -0.7773 0.5998 0.0793 0.028 Uiso 1 1 calc R U
C2 C -0.6493(5) 0.6836(4) -0.0742(4) 0.0273(8) Uani 1 1 d . .
H2A H -0.6039 0.6183 -0.1168 0.033 Uiso 1 1 calc R U
C3 C -0.6342(5) 0.8077(4) -0.1061(3) 0.0263(8) Uani 1 1 d . .
H3A H -0.5758 0.8437 -0.1750 0.032 Uiso 1 1 calc R U
C4 C -0.7448(4) 0.9955(3) -0.0025(3) 0.0189(7) Uani 1 1 d . .
C5 C -0.6895(5) 1.0947(4) -0.0816(3) 0.0260(8) Uani 1 1 d . .
H5A H -0.6303 1.0832 -0.1547 0.031 Uiso 1 1 calc R U
C6 C -0.7272(6) 1.2132(4) -0.0460(4) 0.0303(9) Uani 1 1 d . .
H6A H -0.6897 1.2816 -0.0959 0.036 Uiso 1 1 calc R U
C7 C -0.8185(5) 1.2311(4) 0.0612(4) 0.0264(8) Uani 1 1 d . .
H7A H -0.8438 1.3102 0.0842 0.032 Uiso 1 1 calc R U
C8 C -0.8709(5) 1.1265(3) 0.1329(3) 0.0177(6) Uani 1 1 d . .
C9 C -1.0499(5) 1.2180(4) 0.3040(4) 0.0252(8) Uani 1 1 d . .
H9A H -1.0378 1.3023 0.2865 0.030 Uiso 1 1 calc R U
C10 C -1.1474(5) 1.1651(4) 0.3975(4) 0.0288(8) Uani 1 1 d . .
H10A H -1.2143 1.2055 0.4565 0.035 Uiso 1 1 calc R U
C11 C -1.1265(5) 1.0369(4) 0.3872(3) 0.0241(7) Uani 1 1 d . .
H11A H -1.1798 0.9777 0.4393 0.029 Uiso 1 1 calc R U
N1 N -0.7916(4) 0.7862(3) 0.0710(3) 0.0178(6) Uani 1 1 d . .
N2 N -1.0202(4) 1.0121(3) 0.2925(3) 0.0187(6) Uani 1 1 d . .
N3 N -0.8314(4) 1.0125(3) 0.1015(3) 0.0168(5) Uani 1 1 d . .
N4 N -0.9731(4) 1.1250(3) 0.2405(3) 0.0193(6) Uani 1 1 d . .
N5 N -0.7209(4) 0.8694(3) -0.0180(3) 0.0191(6) 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'
Cu Cu 0.3201 1.2651 '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
O5 Mo1 O2 103.16(12) . .
O5 Mo1 O7 98.58(11) . 2_566
O2 Mo1 O7 100.26(10) . 2_566
O5 Mo1 O3 99.04(10) . .
O2 Mo1 O3 85.42(10) . .
O7 Mo1 O3 159.72(10) 2_566 .
O5 Mo1 O6 92.97(11) . .
O2 Mo1 O6 155.40(10) . .
O7 Mo1 O6 95.47(9) 2_566 .
O3 Mo1 O6 73.66(9) . .
O5 Mo1 O6 164.62(10) . 2_566
O2 Mo1 O6 91.84(10) . 2_566
O7 Mo1 O6 75.05(9) 2_566 2_566
O3 Mo1 O6 85.38(8) . 2_566
O6 Mo1 O6 74.03(9) . 2_566
O4 Mo2 O1 103.97(13) . .
O4 Mo2 O3 100.94(11) . 2_466
O1 Mo2 O3 94.73(11) . 2_466
O4 Mo2 O7 89.52(11) . .
O1 Mo2 O7 100.36(10) . .
O3 Mo2 O7 159.03(10) 2_466 .
O4 Mo2 O8 157.81(10) . .
O1 Mo2 O8 92.75(10) . .
O3 Mo2 O8 91.96(9) 2_466 .
O7 Mo2 O8 72.97(9) . .
O4 Mo2 O8 92.95(11) . 2_466
O1 Mo2 O8 161.45(10) . 2_466
O3 Mo2 O8 74.31(9) 2_466 2_466
O7 Mo2 O8 87.15(8) . 2_466
O8 Mo2 O8 73.10(9) . 2_466
O9 Mo3 O10 103.62(13) . .
O9 Mo3 O8 104.79(11) . .
O10 Mo3 O8 103.59(11) . .
O9 Mo3 O6 102.27(11) . .
O10 Mo3 O6 102.27(11) . .
O8 Mo3 O6 136.54(10) . .
O9 Mo3 O3 89.83(11) . .
O10 Mo3 O3 166.37(11) . .
O8 Mo3 O3 74.48(9) . .
O6 Mo3 O3 72.23(8) . .
O9 Mo3 O7 168.32(11) . .
O10 Mo3 O7 88.01(11) . .
O8 Mo3 O7 72.99(9) . .
O6 Mo3 O7 73.65(8) . .
O3 Mo3 O7 78.50(9) . .
O2 Cu1 N3 166.18(11) 2_466 .
O2 Cu1 N2 97.18(12) 2_466 .
N3 Cu1 N2 79.07(13) . .
O2 Cu1 N1 102.00(12) 2_466 .
N3 Cu1 N1 78.99(12) . .
N2 Cu1 N1 156.27(12) . .
O2 Cu1 O1 92.99(10) 2_466 .
N3 Cu1 O1 100.83(11) . .
N2 Cu1 O1 105.69(11) . .
N1 Cu1 O1 87.25(11) . .
Mo2 O1 Cu1 128.56(13) . .
Mo1 O2 Cu1 147.75(14) . 2_466
Mo2 O3 Mo1 154.23(13) 2_466 .
Mo2 O3 Mo3 104.09(10) 2_466 .
Mo1 O3 Mo3 100.75(9) . .
Mo3 O6 Mo1 107.56(10) . .
Mo3 O6 Mo1 103.07(9) . 2_566
Mo1 O6 Mo1 105.97(9) . 2_566
Mo1 O7 Mo2 152.64(13) 2_566 .
Mo1 O7 Mo3 105.92(10) 2_566 .
Mo2 O7 Mo3 101.41(9) . .
Mo3 O8 Mo2 108.12(10) . .
Mo3 O8 Mo2 102.92(10) . 2_466
Mo2 O8 Mo2 106.90(9) . 2_466
N1 C1 C2 111.1(3) . .
C3 C2 C1 105.8(3) . .
N5 C3 C2 107.1(3) . .
N3 C4 C5 121.7(3) . .
N3 C4 N5 111.5(3) . .
C5 C4 N5 126.8(3) . .
C4 C5 C6 116.5(4) . .
C7 C6 C5 121.8(3) . .
C6 C7 C8 117.2(4) . .
N3 C8 C7 121.5(3) . .
N3 C8 N4 111.6(3) . .
C7 C8 N4 126.8(3) . .
C10 C9 N4 107.5(3) . .
C9 C10 C11 106.1(3) . .
N2 C11 C10 110.4(3) . .
C1 N1 N5 105.2(3) . .
C1 N1 Cu1 142.2(3) . .
N5 N1 Cu1 112.2(2) . .
C11 N2 N4 105.8(3) . .
C11 N2 Cu1 141.3(3) . .
N4 N2 Cu1 112.9(2) . .
C8 N3 C4 121.2(3) . .
C8 N3 Cu1 119.0(2) . .
C4 N3 Cu1 119.8(2) . .
C9 N4 N2 110.3(3) . .
C9 N4 C8 132.7(3) . .
N2 N4 C8 116.8(3) . .
C3 N5 N1 110.7(3) . .
C3 N5 C4 132.0(3) . .
N1 N5 C4 117.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O5 1.700(3) .
Mo1 O2 1.766(2) .
Mo1 O7 1.880(2) 2_566
Mo1 O3 2.028(3) .
Mo1 O6 2.078(2) .
Mo1 O6 2.282(2) 2_566
Mo2 O4 1.705(3) .
Mo2 O1 1.728(2) .
Mo2 O3 1.911(2) 2_466
Mo2 O7 2.032(2) .
Mo2 O8 2.196(2) .
Mo2 O8 2.220(2) 2_466
Mo3 O9 1.705(3) .
Mo3 O10 1.727(3) .
Mo3 O8 1.926(2) .
Mo3 O6 1.962(2) .
Mo3 O3 2.202(2) .
Mo3 O7 2.280(2) .
Cu1 O2 1.894(2) 2_466
Cu1 N3 1.948(3) .
Cu1 N2 1.986(3) .
Cu1 N1 2.014(3) .
Cu1 O1 2.347(3) .
O2 Cu1 1.894(2) 2_466
O3 Mo2 1.911(2) 2_466
O6 Mo1 2.282(2) 2_566
O7 Mo1 1.880(2) 2_566
O8 Mo2 2.220(2) 2_466
C1 N1 1.324(5) .
C1 C2 1.405(5) .
C2 C3 1.363(6) .
C3 N5 1.362(5) .
C4 N3 1.331(4) .
C4 C5 1.383(5) .
C4 N5 1.398(5) .
C5 C6 1.399(6) .
C6 C7 1.379(6) .
C7 C8 1.383(5) .
C8 N3 1.330(4) .
C8 N4 1.394(5) .
C9 C10 1.357(6) .
C9 N4 1.361(5) .
C10 C11 1.405(5) .
C11 N2 1.328(5) .
N1 N5 1.379(4) .
N2 N4 1.374(4) .
