Assembly, structures and properties of polyoxometalate-based supramolecular complexes involving in situ transformation of single-branch N-donor cyano ligands
Wang, Xiang; Li, Yunhui; Zhang, Tong; Ma, Sijia; Wang, Xiuli; CrystEngComm 23 (2021) 3477–3487; doi:10.1039/D1CE00298H

data_7242632
_publ_section_title
;
 Assembly, structures and properties of polyoxometalate-based
 supramolecular complexes involving in situ transformation of
 single-branch N-donor cyano ligands
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3477
_journal_page_last               3487
_journal_paper_doi               10.1039/D1CE00298H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C120 H102 Cu4 Mo12 N16 O60 Si'
_chemical_formula_sum            'C120 H102 Cu4 Mo12 N16 O60 Si'
_chemical_formula_weight         4161.70
_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             2021-01-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-07 deposited with the CCDC.	2021-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                98.7810(10)
_cell_angle_beta                 92.7230(10)
_cell_angle_gamma                112.2170(10)
_cell_formula_units_Z            1
_cell_length_a                   14.4073(6)
_cell_length_b                   14.6547(6)
_cell_length_c                   18.0891(8)
_cell_measurement_reflns_used    4717
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     3471.1(3)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26293
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.537
_diffrn_reflns_theta_min         1.527
_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
_exptl_absorpt_coefficient_mu    1.750
_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    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.772
_refine_diff_density_min         -1.825
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         17493
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+41.0608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11761
_reflns_number_total             17493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00298h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7242631--7242636.cif.'
_cod_database_code               7242632
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O38 \\sim Mo6 \\sim Mo2: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.01 within 2A
O44 \\sim Mo8 \\sim Mo10: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.01 within 2A
C116 \\sim N16 \\sim C92: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.01 within 2A
Uanis(O48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Mo12(0.5) O56(0.5) O60(0.5) O62(0.5) O64(0.5) Mo1(0.5)
4.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C46(H46A,H46B), C54(H54A,H54B), C116(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C16(H16), C22(H22), C28(H28), C30(H30), C36(H36), C38(H38),
 C42(H42A), C44(H44), C48(H48), C50(H50A), C52(H52), C58(H58), C60(H60),
 C62(H62), C68(H68), C76(H76), C78(H78), C80(H80), C84(H84), C86(H86), C88(H88),
  C90(H90), C94(H94), C96(H96), C98(H98), C100(H100), C102(H102), C106(H106),
 C108(H108), C110(H110), C112(H112), C114(H114), C118(H118), C120(H120)
4.d Idealised tetrahedral OH refined as rotating group:
 O18(H18), O42(H42), O50(H50)
;
_shelx_res_checksum              23484
_shelx_hkl_checksum              85265
_olex2_submission_special_instructions 'No special instructions were received'