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_7242634
_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         'C32 H24 Co2 N8 O44 Si W12, 4(O0.50), O'
_chemical_formula_sum            'C32 H24 Co2 N8 O48 Si W12'
_chemical_formula_weight         3640.62
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-21
_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                77.379(2)
_cell_angle_beta                 70.498(2)
_cell_angle_gamma                88.223(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2593(9)
_cell_length_b                   12.2095(10)
_cell_length_c                   12.6834(11)
_cell_measurement_reflns_used    3661
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.16
_cell_volume                     1602.2(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_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       -13
_diffrn_reflns_number            9196
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.711
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    22.072
_exptl_absorpt_correction_T_max  0.137
_exptl_absorpt_correction_T_min  0.106
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    3.773
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.685
_refine_diff_density_min         -3.394
_refine_diff_density_rms         0.320
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         5632
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0835P)^2^+59.3380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4992
_reflns_number_total             5643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00298h2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7242631--7242636.cif.'
_cod_database_code               7242634
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O11) \\sim
Ueq, Uanis(O20) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O4WA) \\sim Ueq,
Uanis(O21) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C13)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(W2B)=1-FVAR(1)
 Sof(W2A)=FVAR(1)
 Sof(W6BB)=1-FVAR(2)
 Sof(W6BA)=FVAR(2)
 Fixed Sof: O1(0.5) W5(0.75) O5(0.5) O7(0.5) O11(0.5) O22(0.5) O21(0.5)
 O20(0.5) O3WB(0.5) O4WA(0.5) O4WB(0.5) O3WA(0.5) O24(0.5) O25(0.5) O26(0.5)
 W2(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16),
 C15(H15)
;
_shelx_res_checksum              63527
_shelx_hkl_checksum              30300
_olex2_submission_special_instructions 'No special instructions were received'