Crystal-to-crystal polymerisation of monosubstituted [PW<sub>11</sub>O<sub>39</sub>Cu(H<sub>2</sub>O)]<sup>5-</sup> Keggin-type anions.
Ruiz-Bilbao, Estibaliz; Pache, Aroa; Barrenechea, Unai; Reinoso, Santiago; San Felices, Leire; Vivanco, Maria dM; Lezama, Luis; Artetxe, Beñat; Gutiérrez-Zorrilla, Juan M; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9042–9051; doi:10.1039/d4dt00690a

data_7716020
_publ_section_title
;
 Crystal-to-crystal polymerisation of monosubstituted
 [PW<sub>11</sub>O<sub>39</sub>Cu(H<sub>2</sub>O)]<sup>5-</sup>
 Keggin-type anions.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9042
_journal_page_last               9051
_journal_paper_doi               10.1039/d4dt00690a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'Cu1 O39 P W11, C6 H4 Cu0.5 N O2, O, 4(C H6 N3), C H5 N2.5'
_chemical_formula_sum            'C11 H36 Cu1.5 N16 O42 P W11'
_chemical_formula_weight         3213.19
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-11-30T18:17:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2024-05-02 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.490(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1291(5)
_cell_length_b                   19.1015(7)
_cell_length_c                   20.7513(9)
_cell_measurement_reflns_used    7680
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      27.819
_cell_measurement_theta_min      2.163
_cell_volume                     5194.5(4)
_computing_cell_refinement
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
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        CrysAlisPro, Agilent Technologies,
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_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
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_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector_area_resol_mean 16.2439
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0399123
_diffrn_orient_matrix_UB_12      0.0249079
_diffrn_orient_matrix_UB_13      0.0015327
_diffrn_orient_matrix_UB_21      -0.0311805
_diffrn_orient_matrix_UB_22      -0.020553
_diffrn_orient_matrix_UB_23      -0.021804
_diffrn_orient_matrix_UB_31      -0.0191563
_diffrn_orient_matrix_UB_32      -0.0183361
_diffrn_orient_matrix_UB_33      0.0263409
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0956
_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       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23098
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         1.885
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.996
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.35544
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    4.109
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5690
_exptl_crystal_size_max          0.3126
_exptl_crystal_size_mid          0.2396
_exptl_crystal_size_min          0.1993
_refine_diff_density_max         5.832
_refine_diff_density_min         -2.561
_refine_diff_density_rms         0.527
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         10213
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+352.9782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2437
_reflns_Friedel_coverage         0
_reflns_number_gt                6861
_reflns_number_total             10213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00690a2.cif
_cod_data_source_block           a2014200_ar624ht_reh10dias
_cod_depositor_comments
'Adding full bibliography for 7716020--7716022.cif.'
_cod_original_formula_sum        'C11 H36 Cu1.50 N16 O42 P W11'
_cod_database_code               7716020