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_7242636
_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 H96 Cu4 Mo12 N16 O56 Si, C60 H48 Cu2 Mo12 N8 O48 Si, 6(H2 O), 2(C15 H12 N2 O2)'
_chemical_formula_sum            'C210 H178 Cu6 Mo24 N28 O114 Si2'
_chemical_formula_weight         7659.87
_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
_audit_creation_date             2021-01-21
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-07 deposited with the CCDC.	2021-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                67.6880(10)
_cell_angle_beta                 71.6510(10)
_cell_angle_gamma                66.9130(10)
_cell_formula_units_Z            1
_cell_length_a                   16.2488(10)
_cell_length_b                   19.1465(12)
_cell_length_c                   24.0881(14)
_cell_measurement_reflns_used    5054
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     6255.3(7)
_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  'ShelXL (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36325
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.082
_diffrn_reflns_theta_max         25.082
_diffrn_reflns_theta_min         0.932
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_correction_T_min  0.661
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3758
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.500
_refine_diff_density_min         -1.848
_refine_diff_density_rms         0.149
_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     1760
_refine_ls_number_reflns         22191
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0573P)^2^+37.4936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13975
_reflns_number_total             22221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00298h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7242631--7242636.cif.'
_cod_database_code               7242636
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.719
_shelx_estimated_absorpt_t_min   0.677
_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. Restrained distances
 C85-C105
 1.54 with sigma of 0.01
 H1WA-H2WB
 2.08 with sigma of 0.02
 O59-C96 = O57-C75 = O60-C105
 1.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C103 \\sim C104 \\sim C102: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C99 \\sim C104 \\sim C100: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C92 \\sim C91 \\sim C95: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C95 \\sim C63: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O22 \\sim O25 \\sim O39 \\sim O48 \\sim O50 \\sim O52: within 3.8A with sigma
of 0.005 and sigma for terminal atoms of 0.01
O25 \\sim Mo7 \\sim Mo5: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.01
O50 \\sim Mo10 \\sim Mo12: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.01
Uanis(Mo11) \\sim Ueq, Uanis(Mo12) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C104)
\\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C102) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O29(0.5) O42(0.5) O43(0.5) O44(0.5) O45(0.5) O46(0.5) O47(0.5)
 O51(0.5)
5.a Free rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C11(H11A,H11B), C13(H13A,H13B), C29(H29A,H29B), C76(H76A,H76B),
 C77(H77A,H77B), C97(H97A,H97B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C12(H12), C14(H14), C16(H16), C18(H18), C19(H19),
 C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C30(H30), C31(H31), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C42(H42),
 C44(H44), C45(H45), C46(H46), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
  C55(H55), C58(H58), C60(H60), C61(H61), C65(H65), C66(H66), C67(H67),
 C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C79(H79), C80(H80),
  C81(H81), C82(H82), C83(H83), C84(H84), C86(H86), C87(H87), C89(H89),
 C90(H90), C92(H92), C93(H93), C94(H94), C95(H95), C98(H98), C99(H99),
 C100(H100), C103(H103), C104(H104)
5.d Fitted hexagon refined as free rotating group:
 C85(C86,C87,C88,C89,C90), C99(C100,C101,C102,C103,C104)
5.e Idealised tetrahedral OH refined as rotating group:
 O32(H32), O41(H41), O49(H49A), O54(H54), O55(H55A), O59(H59), O60(H60A)
;
_shelx_res_checksum              88495
_shelx_hkl_checksum              41361
_olex2_submission_special_instructions 'No special instructions were received'