Magneto-structural correlations of cyclo-tetravanadates functionalized with mixed-ligand copper(ii) complexes
Sánchez-Lara, Eduardo; García-García, Amalia; González-Vergara, Enrique; Cepeda, Javier; Rodríguez-Diéguez, Antonio; New Journal of Chemistry 45 (2021) 5081–5092; doi:10.1039/D0NJ06004F

data_7060392
_publ_section_title
;
 Magneto-structural correlations of cyclo-tetravanadates functionalized
 with mixed-ligand copper(ii) complexes
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5081
_journal_page_last               5092
_journal_paper_doi               10.1039/D0NJ06004F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         '2(C16 H22 Cu N4 O8 V2), 7(H2 O)'
_chemical_formula_sum            'C32 H58 Cu2 N8 O23 V4'
_chemical_formula_weight         1253.70
_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
_audit_creation_date             2019-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-12 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                98.0718(16)
_cell_angle_beta                 108.6313(19)
_cell_angle_gamma                92.8695(18)
_cell_formula_units_Z            2
_cell_length_a                   11.9013(3)
_cell_length_b                   12.1828(2)
_cell_length_c                   18.2260(3)
_cell_measurement_reflns_used    26797
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5380
_cell_measurement_theta_min      3.1940
_cell_volume                     2466.59(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5564
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -115.00 -57.00   1.00   10.02    --  -24.73-178.00-150.00   58
  2  \w   -115.00 -57.00   1.00   10.02    --  -24.73-178.00 -30.00   58
  3  \w   -115.00 -57.00   1.00   10.02    --  -24.73-178.00  90.00   58
  4  \w      0.00 103.00   1.00   10.02    --   26.76  38.00  60.00  103
  5  \w     -7.00 105.00   1.00   10.02    --   26.76  77.00  60.00  112
  6  \w     35.00 117.00   1.00   10.02    --   26.76 178.00 -90.00   82
  7  \w    -47.00  56.00   1.00   10.02    --   26.76 -57.00 -90.00  103
  8  \w    -25.00  69.00   1.00   10.02    --   26.76 -99.00 150.00   94
  9  \w     32.00 115.00   1.00   10.02    --   26.76-178.00-120.00   83
 10  \w     -7.00 105.00   1.00   10.02    --   26.76  77.00 -90.00  112
 11  \w   -113.00 -53.00   1.00   10.02    --  -24.73 178.00 150.00   60
 12  \w    -99.00   5.00   1.00   10.02    --  -24.73 -57.00 -90.00  104
 13  \w     -7.00 105.00   1.00   10.02    --   26.76  77.00-120.00  112
 14  \w     -3.00 101.00   1.00   10.02    --   26.76  57.00-180.00  104
 15  \w    -25.00  69.00   1.00   10.02    --   26.76 -99.00   0.00   94
 16  \w    -25.00  69.00   1.00   10.02    --   26.76 -99.00  60.00   94
 17  \w     35.00 117.00   1.00   10.02    --   26.76 178.00 150.00   82
 18  \w    -25.00  69.00   1.00   10.02    --   26.76 -99.00-120.00   94
 19  \w    -19.00 108.00   1.00   10.02    --   26.76  19.00-150.00  127
 20  \w      0.00 103.00   1.00   10.02    --   26.76  38.00  90.00  103
 21  \w      0.00 103.00   1.00   10.02    --   26.76  38.00-150.00  103
 22  \w    -63.00 116.00   1.00   10.02    --   26.76   0.00-150.00  179
 23  \w    -63.00   5.00   1.00   10.02    --   26.76   0.00-120.00   68
 24  \w    -63.00 116.00   1.00   10.02    --   26.76   0.00-180.00  179
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0569803000
_diffrn_orient_matrix_UB_12      -0.0200668000
_diffrn_orient_matrix_UB_13      0.0105846000
_diffrn_orient_matrix_UB_21      -0.0254429000
_diffrn_orient_matrix_UB_22      -0.0523709000
_diffrn_orient_matrix_UB_23      -0.0234826000
_diffrn_orient_matrix_UB_31      0.0101268000
_diffrn_orient_matrix_UB_32      0.0186627000
_diffrn_orient_matrix_UB_33      -0.0327196000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            83873
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         8700
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0415P)^2^+9.0430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7676
_reflns_number_total             8700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj06004f2.cif
_cod_data_source_block           ov_aml-403_mo
_cod_depositor_comments
'Adding full bibliography for 7060390--7060392.cif.'
_cod_database_code               7060392
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H58Cu2N8O23V4
_cell_oxdiff_angle_alpha         98.0718(16)
_cell_oxdiff_angle_beta          108.6313(19)
_cell_oxdiff_angle_gamma         92.8695(18)
_cell_oxdiff_length_a            11.9013(3)
_cell_oxdiff_length_b            12.1828(2)
_cell_oxdiff_length_c            18.2260(3)
_cell_oxdiff_measurement_reflns_used 26797
_cell_oxdiff_volume              2466.59(9)
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H)
  groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups, All N(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C30A-C31A \\sim C30B-C31B
 with sigma of 0.02
 C32B-C31B \\sim C32A-C31A
 with sigma of 0.02
 C33-C32A \\sim C32B-C33
 with sigma of 0.02
 C30B-C29 \\sim C29-C30A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N17) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C32B) = Uanis(C32A)
Uanis(C31B) = Uanis(C31A)
Uanis(C30B) = Uanis(C30A)
Uanis(C15A) = Uanis(C15B)
4. Rigid body (RIGU) restrains
 C29, C30B, C31B, C32B, C33, N34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11, C12B, C13B, C16A, C14B, C15A, O8B, O7B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11, C12A, N17, C13A, C14A, C16B, C15B, O7A, O8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H3BC)=Sof(H3BD)=Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(H13A)=Sof(H13B)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C14B)=
 Sof(H14C)=Sof(H14D)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(O8B)=Sof(O7B)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C12A)=Sof(H12A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=
 Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(O7A)=Sof(O8A)=FVAR(1)
 Sof(H29A)=Sof(C30B)=Sof(H30A)=Sof(H30B)=Sof(H33C)=Sof(H33D)=Sof(C31B)=
 Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=1-FVAR(2)
 Sof(H29)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(H33A)=Sof(H33B)=Sof(C31A)=
 Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=FVAR(2)
6.a Free rotating group:
 O17(H17G,H17H), O22(H22A,H22B), O23(H23A,H23B), O19(H19A,H19B), O18(H18A,
 H18B), O20(H20A,H20B), O21(H21A,H21B)
6.b Ternary CH refined with riding coordinates:
 C12B(H12B), C12A(H12A), C29(H29A), C29(H29)
6.c Secondary CH2 refined with riding coordinates:
 N3(H3BC,H3BD), N3(H3AA,H3AB), N6(H6A,H6B), C13B(H13A,H13B), C16A(H16A,H16B),
 C13A(H13C,H13D), C14A(H14A,H14B), C16B(H16C,H16D), C14B(H14C,H14D), C15A(H15A,
 H15B), C15B(H15C,H15D), C30B(H30A,H30B), C30A(H30C,H30D), C33(H33A,H33B),
 C33(H33C,H33D), C31A(H31A,H31B), C31B(H31C,H31D), C32A(H32A,H32B), C32B(H32C,
 H32D)
6.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C7(H7), C8(H8), C2(H2), C9(H9), C4(H4), C24(H24), C27(H27),
 C26(H26), C18(H18), C3(H3), C21(H21), C20(H20), C19(H19), C25(H25)
6.e Idealised Me refined as rotating group:
 N17(H17A,H17B,H17C), N17(H17D,H17E,H17F), N34(H34A,H34B,H34C)
;
_shelx_res_checksum              35337
_shelx_hkl_checksum              30154
_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 6.608
_oxdiff_exptl_absorpt_empirical_full_min 0.626