A trapped hexaaqua Co<sup>II</sup> complex between the polyanionic sheets of decavanadate reveals high axial anisotropy and field induced SIM behaviour.
Sahu, Pradip Kumar; Mondal, Arpan; Konar, Sanjit; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3825–3831; doi:10.1039/d0dt04339g

data_7706568
_publ_section_title
;
 A trapped hexaaqua Co<sup>II</sup> complex between the polyanionic sheets
 of decavanadate reveals high axial anisotropy and field induced SIM
 behaviour.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3825
_journal_page_last               3831
_journal_paper_doi               10.1039/d0dt04339g
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'Co H12 O6, H28 Na4 O42 V10, 4(H2 O)'
_chemical_formula_sum            'Co H48 Na4 O52 V10'
_chemical_formula_weight         1540.67
_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     iterative
_audit_creation_date             2020-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-11 deposited with the CCDC.	2021-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                105.173(2)
_cell_angle_beta                 97.581(2)
_cell_angle_gamma                100.899(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0156(6)
_cell_length_b                   11.2788(7)
_cell_length_c                   11.6948(8)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.34
_cell_volume                     1106.19(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      140.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23961
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.436
_diffrn_reflns_theta_min         2.344
_exptl_absorpt_coefficient_mu    2.549
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.313
_exptl_crystal_description       cubic
_exptl_crystal_F_000             765
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4549
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0259P)^2^+3.2096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3994
_reflns_number_total             4549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04339g2.cif
_cod_data_source_block           ps_a
_cod_depositor_comments          'Adding full bibliography for 7706568.cif.'
_cod_database_code               7706568
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H23A,H23B} of O23, {H21A,H21B} of O21, {H24A,H24B} of O24, {H18A,H18B} of O18
 At 1.5 times of:
  {H26A,H26B} of O26, {H2A,H2B} of O2, {H25A,H25B} of O25, {H22A,H22B} of O22,
   {H1A,H1B} of O1, {H27A,H27B} of O27, {H19A,H19B} of O19, {H3A,H3B} of O3,
  {H20A,H20B} of O20
2. Restrained distances
 Na2-H19A \\sim Na2-H19B
 with sigma of 0.02
 Co1-H1A \\sim Co1-H1B
 with sigma of 0.02
3. Others
 Fixed Sof: O27(0.65) H27A(0.65) H27B(0.65) O26(0.35) H26A(0.35) H26B(0.35)
4.a Free rotating group:
 O25(H25A,H25B), O19(H19A,H19B), O1(H1A,H1B), O27(H27A,H27B), O26(H26A,H26B)
4.b Rotating group:
 O2(H2A,H2B), O3(H3A,H3B), O22(H22A,H22B), O20(H20A,H20B)
4.c Secondary CH2 refined with riding coordinates:
 O23(H23A,H23B), O21(H21A,H21B), O18(H18A,H18B), O24(H24A,H24B)
;
_shelx_res_checksum              97316
_shelx_hkl_checksum              55314
_olex2_submission_special_instructions 'No special instructions were received'