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_7060391
_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         'C34 H40 Cu2 N8 O16 V4, 6(H2 O)'
_chemical_formula_sum            'C34 H52 Cu2 N8 O22 V4'
_chemical_formula_weight         1255.67
_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
_audit_creation_date             2017-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-11-12 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                70.470(3)
_cell_angle_beta                 73.209(3)
_cell_angle_gamma                80.836(3)
_cell_formula_units_Z            1
_cell_length_a                   8.9373(3)
_cell_length_b                   11.4902(4)
_cell_length_c                   12.9580(4)
_cell_measurement_reflns_used    7258
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5160
_cell_measurement_theta_min      3.2910
_cell_volume                     1197.75(7)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26431
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.917
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87097
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       prism
_exptl_crystal_F_000             638
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         4904
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0538P)^2^+3.7280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3994
_reflns_number_total             4904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj06004f2.cif
_cod_data_source_block           lolacuv_1_mo
_cod_depositor_comments
'Adding full bibliography for 7060390--7060392.cif.'
_cod_database_code               7060391
_shelx_shelxl_version_number     2016/6
_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,H,H)
  groups
 At 1.5 times of:
  All N(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9A = O9-H9B
 0.85 with sigma of 0.02
 H9A-H9B
 1.34 with sigma of 0.04
 O10-H10A = O10-H10B
 0.85 with sigma of 0.02
 H10A-H10B
 1.34 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=
 Sof(H4BC)=Sof(H4BD)=Sof(H1BC)=Sof(H1BD)=Sof(H4BF)=Sof(H4BG)=Sof(H4BH)=1-FVAR(1)
 Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 Sof(H4AA)=Sof(H4AB)=Sof(H1AA)=Sof(H1AB)=Sof(H4AC)=Sof(H4AD)=Sof(H4AE)=FVAR(1)
6.a Riding coordinates:
 O11(H11A,H11B)
6.b Ternary CH refined with riding coordinates:
 C2A(H2A), C2B(H2B)
6.c Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C5A(H5AA,H5AB), C3B(H3BA,H3BB), C5B(H5BA,H5BB), C4(H4AA,H4AB),
  C4(H4BC,H4BD), N1(H1AA,H1AB), N1(H1BC,H1BD)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15)
6.e Idealised Me refined as rotating group:
 N4(H4AC,H4AD,H4AE), N4(H4BF,H4BG,H4BH)
;
_shelx_res_checksum              69853
_shelx_hkl_checksum              18159
_olex2_submission_special_instructions 'No special instructions were received'