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_7716022
_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
'C6 H4 Cu1.5 N O42 P W11, 5(O), 4.5(C H6 N3), C0.5 H2.5 N1.5'
_chemical_formula_sum            'C11 H46 Cu1.5 N16 O47 P W11'
_chemical_formula_weight         3303.27
_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             2024-05-02T12:57:05-00:00
_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                 93.8906(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.96551(18)
_cell_length_b                   21.5917(3)
_cell_length_c                   22.2169(3)
_cell_measurement_reflns_used    46463
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      30.038
_cell_measurement_theta_min      2.055
_cell_volume                     5726.63(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0141268
_diffrn_orient_matrix_UB_12      0.0182367
_diffrn_orient_matrix_UB_13      -0.0249297
_diffrn_orient_matrix_UB_21      0.002553
_diffrn_orient_matrix_UB_22      -0.0271334
_diffrn_orient_matrix_UB_23      -0.0178547
_diffrn_orient_matrix_UB_31      -0.0576562
_diffrn_orient_matrix_UB_32      0.0032693
_diffrn_orient_matrix_UB_33      -0.0091307
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71075
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.349
_diffrn_reflns_theta_min         1.886
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    22.685
_exptl_absorpt_correction_T_max  0.374
_exptl_absorpt_correction_T_min  0.069
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
        Numerical absorption correction based on gaussian integration over
        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.831
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5890
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.063
_refine_diff_density_max         2.032
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         11677
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0107P)^2^+64.5108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0
_reflns_number_gt                10170
_reflns_number_total             11677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00690a2.cif
_cod_data_source_block           b20240088_p2agudumo_auto
_cod_depositor_comments
'Adding full bibliography for 7716020--7716022.cif.'
_cod_original_cell_volume        5726.65(15)
_cod_original_formula_sum        'C11 H46 Cu1.50 N16 O47 P W11'
_cod_database_code               7716022