Two polymolybdate-directed Zn(ii) complexes tuned by a new bis-pyridine-bis-amide ligand with a diphenylketone spacer for efficient ampere sensing and dye adsorption
Wang, Xiu-Li; Zhang, Yue; Chen, Yong-Zhen; Wang, Yue; Wang, Xiang; CrystEngComm  (2022) –; doi:10.1039/D2CE00697A

data_7245141
_publ_section_title
;
 Two polymolybdate-directed Zn(ii) complexes tuned by a new
 bis-pyridine-bis-amide ligand with a diphenylketone spacer for efficient
 ampere sensing and dye adsorption
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00697A
_journal_year                    2022
_chemical_formula_moiety
'C50 H40 Cr2 Mo12 N8 O56 Zn, Cr2 H8 Mo12 O52 Zn, 4(C25 H18 N4 O3), 4(H2 O), 3.5(O)'
_chemical_formula_sum            'C150 H128 Cr4 Mo24 N24 O128 Zn2'
_chemical_formula_weight         6956.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-09
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-04 deposited with the CCDC.	2022-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                81.3870(10)
_cell_angle_beta                 76.8240(10)
_cell_angle_gamma                89.5660(10)
_cell_formula_units_Z            1
_cell_length_a                   12.0142(5)
_cell_length_b                   19.6645(9)
_cell_length_c                   22.4864(11)
_cell_measurement_reflns_used    4631
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     5112.3(4)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38346
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.379
_diffrn_reflns_theta_min         0.941
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.965
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.124
_refine_diff_density_min         -2.299
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1511
_refine_ls_number_reflns         25399
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0510
_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/[\s^2^(Fo^2^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15341
_reflns_number_total             25399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00697a2.cif
_cod_data_source_block           2
_cod_original_cell_volume        5112.4(4)
_cod_database_code               7245141
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Zn1-H1WA \\sim Zn1-H1WB
 with sigma of 0.02
 Zn2-H2WA \\sim Zn2-H2WB
 with sigma of 0.02
3. Others
 Fixed Sof: O7W(0.75)
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O5W(H5WA,H5WB), O29(H29A,H29B)
4.b Rotating group:
 O3W(H3WA,H3WB)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N10(H10), N12(H12A), N3(H3), C4(H4), C10(H10A), N9(H9A), C12(H12),
 C14(H14), C24(H24), C30(H30), C32(H32), C38(H38), C40(H40), C42(H42), C44(H44),
  C46(H46), C48(H48), C50(H50), C56(H56), C58(H58), C60(H60), C62(H62),
 C64(H64), C66(H66), C68(H68), C70(H70), C74(H74), C19(H19), C39(H39), C5(H5),
 C41(H41), C43(H43), C45(H45), C47(H47), C3(H3A), C49(H49), C51(H51), C53(H53),
 C27(H27), C7(H7), C57(H57), C59(H59), C15(H15), C63(H63), C2(H2), C65(H65),
 N11(H11), C33(H33), C69(H69), C35(H35), C71(H71), C9(H9), C73(H73)
;
_shelx_res_checksum              49408
_shelx_hkl_checksum              84614
_olex2_submission_special_instructions 'No special instructions were received'