Redox and guest tunable spin-crossover properties in a polymeric polyoxometalate.
Palacios-Corella, Mario; García-López, Víctor; Waerenborgh, Joao Carlos; Vieira, Bruno J. C.; Mínguez Espallargas, Guillermo; Clemente-León, Miguel; Coronado, Eugenio; Chemical science 14 (2023) 3048–3055; doi:10.1039/d2sc05800f

data_1568503
_publ_section_title
;
 Redox and guest tunable spin-crossover properties in a polymeric
 polyoxometalate.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              3048
_journal_page_last               3055
_journal_paper_doi               10.1039/d2sc05800f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C32 H30 N12 O21 V6 Zn, 1.75(C3 H7 N O), C2 H3 N'
_chemical_formula_sum            'C39.25 H45.25 N14.75 O22.75 V6 Zn'
_chemical_formula_weight         1458.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-18
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-19 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.503(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2016(16)
_cell_length_b                   27.457(4)
_cell_length_c                   18.236(2)
_cell_measurement_reflns_used    932
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.0390
_cell_measurement_theta_min      3.8680
_cell_volume                     6369.6(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      393.15
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -82.00   -9.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.8880  -64.0000   53.3253 73

  2 omega  -67.00    4.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.8880  -65.0000  125.5766 71

  3 omega  -83.00    6.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.8880  -68.0000 -127.3603 89

  4 omega  -84.00   -9.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.8880  -57.0000  -30.0000 75

  5 omega  -45.00   40.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       15.6692  -67.0000    8.8736 85

  6 omega  -34.00   40.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       15.6692  -67.0000 -163.7472 74

  7 omega  -47.00   40.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       15.6692  -67.0000  -62.6868 87

  8 omega  -49.00   40.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       15.6692  -67.0000  115.2813 89
;
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3828
_diffrn_reflns_av_unetI/netI     0.2483
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51146
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        20.814
_diffrn_reflns_theta_max         20.814
_diffrn_reflns_theta_min         3.237
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.2169
_refine_ls_R_factor_gt           0.1233
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1492P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2764
_refine_ls_wR_factor_ref         0.3306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2989
_reflns_number_total             6645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05800f2.cif
_cod_data_source_block           polzn1a
_cod_depositor_comments
'Adding full bibliography for 1568503--1568506.cif.'
_cod_original_cell_volume        6369.8(15)
_cod_database_code               1568503
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.801
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C22S(0.75) H22C(0.75) H22D(0.75) H22E(0.75) N21S(0.75) C23S(0.75)
 H23A(0.75) H23B(0.75) H23C(0.75) O25S(0.75) C24S(0.75) H24S(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C20(H20A,H20B), C52(H52A,H52B), C50(H50A,
 H50B), C51(H51A,H51B)
3.b Me refined with riding coordinates:
 C22S(H22C,H22D,H22E), C12S(H12A,H12B,H12C), C13S(H13A,H13B,H13C), C23S(H23A,
 H23B,H23C)
3.c Aromatic/amide H refined with riding coordinates:
 N48(H48), C41(H41), N18(H18), C3(H3), C14(H14), C11(H11), C15(H15), C40(H40),
 C39(H39), C33(H33), C5(H5), C16(H16), C35(H35), C9(H9), C46(H46), C44(H44),
 C45(H45), C10(H10), C14S(H14S), C24S(H24S)
3.d Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              84435
_shelx_hkl_checksum              67655
_shelx_fab_checksum              98229
_olex2_submission_special_instructions 'No special instructions were received'