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_1568504
_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 H32 N12 O21 V6, 2(C10 H10 Co), 4(C2 H3 N)'
_chemical_formula_sum            'C60 H64 Co2 N16 O21 V6'
_chemical_formula_weight         1768.77
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-19
_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                79.422(2)
_cell_angle_beta                 80.163(2)
_cell_angle_gamma                76.369(3)
_cell_formula_units_Z            1
_cell_length_a                   9.8603(3)
_cell_length_b                   12.1228(4)
_cell_length_c                   17.2505(4)
_cell_measurement_reflns_used    7808
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.9210
_cell_measurement_theta_min      2.9770
_cell_volume                     1952.25(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -94.00   6.00   1.00    6.50    --  -20.96 -38.00 -30.00  100
  2  \w    -15.00  65.00   1.00    6.50    --   21.90 -99.00-120.00   80
  3  \w    -10.00  42.00   1.00    6.50    --   21.90  77.00   0.00   52
  4  \w    -47.00  44.00   1.00    6.50    --   21.90 -57.00 120.00   91
  5  \w    -47.00  44.00   1.00    6.50    --   21.90 -57.00 -90.00   91
  6  \w    -42.00  54.00   1.00    6.50    --   21.90 -77.00  30.00   96
  7  \w    -10.00  42.00   1.00    6.50    --   21.90  77.00 120.00   52
  8  \w      0.00  91.00   1.00    6.50    --   21.90  57.00 -90.00   91
  9  \w      0.00  91.00   1.00    6.50    --   21.90  57.00-180.00   91
 10  \w    -94.00   2.00   1.00    6.50    --  -20.96 -38.00  60.00   96
 11  \w    -15.00  65.00   1.00    6.50    --   21.90 -99.00  60.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0649155000
_diffrn_orient_matrix_UB_12      -0.0403198000
_diffrn_orient_matrix_UB_13      0.0016588000
_diffrn_orient_matrix_UB_21      0.0091747000
_diffrn_orient_matrix_UB_22      0.0032198000
_diffrn_orient_matrix_UB_23      -0.0419827000
_diffrn_orient_matrix_UB_31      0.0357797000
_diffrn_orient_matrix_UB_32      0.0455157000
_diffrn_orient_matrix_UB_33      -0.0040110000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37801
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.896
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.945
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         10216
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1232P)^2^+6.3281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6918
_reflns_number_total             10216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05800f2.cif
_cod_data_source_block           test_a
_cod_depositor_comments
'Adding full bibliography for 1568503--1568506.cif.'
_cod_database_code               1568504
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.664
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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, All O(H) groups
2. Restrained distances
 O2-H2A
 0.85 with sigma of 0.01
 V2-H2A
 2.227054 with sigma of 0.02
 V1-H2A
 2.561938 with sigma of 0.02
3. Others
 Fixed Sof: C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C28(0.5) N6(0.5) C29(0.5)
 H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5) N7(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 H31C(0.5) C32(0.5) N8(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5)
 N9(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11),
 N00G(H00G), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,H33B,
 H33C)
;
_shelx_res_checksum              3502
_shelx_hkl_checksum              63839
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.218
_oxdiff_exptl_absorpt_empirical_full_min 0.764