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_7060390
_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
'C14 H14 Cu N3 O3, C14 H12 Cu N3 O8 V2, 4(H2 O), H2 O0.786, 0.214(O)'
_chemical_formula_sum            'C28 H36 Cu2 N6 O16 V2'
_chemical_formula_weight         941.59
_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_block_doi                 10.5517/ccdc.csd.cc250hqf
_audit_creation_date             2020-04-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-12 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                109.108(3)
_cell_angle_beta                 95.685(3)
_cell_angle_gamma                113.173(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9249(4)
_cell_length_b                   13.2626(4)
_cell_length_c                   13.5191(4)
_cell_measurement_reflns_used    12971
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.1460
_cell_measurement_theta_min      3.5460
_cell_volume                     1792.27(12)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_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 0.9862
_diffrn_measured_fraction_theta_max 0.9972
_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 -95.00 3.00 1.00 1.91 -- -41.16 125.00 -30.00 98
 2 \w -117.00 -15.00 1.00 1.91 -- -41.16 -38.00 120.00 102
 3 \w -117.00 -15.00 1.00 1.91 -- -41.16 -38.00 30.00 102
 4 \w -95.00 3.00 1.00 1.91 -- -41.16 125.00-180.00 98
 5 \w -115.00 -67.00 1.00 1.91 -- -41.16-134.00 171.00 48
 6 \w 24.00 103.00 1.00 1.91 -- 41.16-134.00 171.00 79
 7 \w 18.00 98.00 1.00 1.91 -- 41.16-125.00 0.00 80
 8 \w 100.00 178.00 1.00 7.63 -- 115.00 111.00 -90.00 78
 9 \w 57.00 178.00 1.00 7.63 -- 115.00 16.00 39.56 121
 10 \w 40.00 147.00 1.00 7.63 -- 115.00 -68.00 -36.01 107
 11 \w 84.00 178.00 1.00 7.63 -- 115.00 30.00 120.00 94
 12 \w 37.00 116.00 1.00 7.63 -- 115.00-111.00 90.00 79
 13 \w 31.00 109.00 1.00 7.63 -- 115.00 -95.00 90.00 78
 14 \w 37.00 116.00 1.00 7.63 -- 115.00-111.00 150.00 79
 15 \w 57.00 150.00 1.00 7.63 -- 115.00 178.00 -90.00 93
 16 \w 85.00 178.00 1.00 7.63 -- 115.00 61.00-180.00 93
 17 \w 37.00 116.00 1.00 7.63 -- 115.00-111.00-150.00 79
 18 \w 37.00 116.00 1.00 7.63 -- 115.00-111.00 -60.00 79
 19 \w 37.00 116.00 1.00 7.63 -- 115.00-111.00 -30.00 79
 20 \w 31.00 109.00 1.00 7.63 -- 115.00 -95.00-180.00 78
 21 \w 100.00 178.00 1.00 7.63 -- 115.00 111.00 150.00 78
 22 \w 37.00 116.00 1.00 7.63 -- 115.00-111.00 -90.00 79
 23 \w 81.00 178.00 1.00 7.63 -- 115.00 77.00 -60.00 97
 24 \w 85.00 178.00 1.00 7.63 -- 115.00 61.00-120.00 93
 25 \w 36.00 149.00 1.00 7.63 -- 115.00 -77.00-120.00 113
 26 \w 31.00 109.00 1.00 7.63 -- 115.00 -95.00-150.00 78
 27 \w 40.00 143.00 1.00 7.63 -- 115.00 -45.00 0.00 103
 28 \w 31.00 109.00 1.00 7.63 -- 115.00 -95.00 -30.00 78
 29 \w 84.00 178.00 1.00 7.63 -- 115.00 30.00-120.00 94
 30 \w 57.00 150.00 1.00 7.63 -- 115.00 178.00-120.00 93
 31 \w 31.00 109.00 1.00 7.63 -- 115.00 -95.00 120.00 78
 32 \w 37.00 146.00 1.00 7.63 -- 115.00 -30.00-120.00 109
 33 \w 31.00 109.00 1.00 7.63 -- 115.00 -95.00 30.00 78
 34 \w 37.00 116.00 1.00 7.63 -- 115.00-111.00 30.00 79
 35 \w 37.00 146.00 1.00 7.63 -- 115.00 -30.00-180.00 109
 36 \w 32.00 176.00 1.00 7.63 -- 115.00 -15.00 120.00 144
 37 \w 99.00 149.00 1.00 7.63 -- 115.00 -82.00-154.37 50
 38 \w 31.00 67.00 1.00 7.63 -- 115.00 -95.00 -60.00 36
 39 \w 72.00 98.00 1.00 7.63 -- 115.00 -95.00 -60.00 26
 40 \w 119.00 145.00 1.00 7.63 -- 115.00 45.00 60.00 26
 41 \w 86.00 116.00 1.00 7.63 -- 115.00 61.00 60.00 30
 42 \w 72.00 98.00 1.00 7.63 -- 115.00 -77.00-180.00 26
 43 \w 34.00 81.00 1.00 7.63 -- 115.00 -82.00-154.37 47
;
_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      0.0734398000
_diffrn_orient_matrix_UB_12      0.0267657000
_diffrn_orient_matrix_UB_13      0.1133180000
_diffrn_orient_matrix_UB_21      -0.0662099000
_diffrn_orient_matrix_UB_22      0.0745528000
_diffrn_orient_matrix_UB_23      0.0527051000
_diffrn_orient_matrix_UB_31      -0.1069102000
_diffrn_orient_matrix_UB_32      -0.1128682000
_diffrn_orient_matrix_UB_33      0.0005437000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38143
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.355
_diffrn_reflns_theta_min         3.586
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.292
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       irregular
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00035(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0495P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6525
_reflns_number_total             7587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj06004f2.cif
_cod_data_source_block           glyfencuv_cu
_cod_depositor_comments
'Adding full bibliography for 7060390--7060392.cif.'
_cod_original_cell_volume        1792.27(10)
_cod_database_code               7060390
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H36N6Cu2V2O16
_chemical_oxdiff_usercomment     'Eduardo Sanchez Lara'
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.252
_reflns_odcompleteness_completeness 98.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.17
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(O13A)=1-FVAR(1)
 Sof(O13)=FVAR(1)
 Sof(O10B)=1-FVAR(2)
 Sof(O10A)=FVAR(2)
 Sof(O8B)=1-FVAR(3)
 Sof(O8A)=FVAR(3)
3.a Free rotating group:
 O12(H12A,H12B), O11(H11A,H11B), O14(H14A,H14B), O10B(H10A,H10B), O13(H13A,H13B)
3.b Rotating group:
 O9(H9A,H9B)
3.c Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), N3(H3A,H3B), C26(H26A,H26B), C28(H28A,H28B)
3.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C22(H22), C18(H18), C13(H13), C1(H1), C21(H21), C17(H17), C9(H9),
 C10(H10), C3(H3), C8(H8), C6(H6), C15(H15), C20(H20), C5(H5), C2(H2)
;
_shelx_res_checksum              44932
_shelx_hkl_checksum              80457
_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 1.567
_oxdiff_exptl_absorpt_empirical_full_min 0.853