Two isostructural complexes of Ni(ii) and Zn(ii) with violurate and pyridine: a detailed structural, theoretical, magnetic, and NMR investigation
Roy, Subhadip; Mal, Susital; Banik, Rupak; Das, Subrata; Dlháň, Ľubor; Titiš, Ján; Boča, Roman; Kirillov, Alexander M.; Novikov, Alexander S.; Hazendonk, Paul; Butcher, Ray J.; Bauza, Antonio; Frontera, Antonio; CrystEngComm 25 (2023) 6503–6511; doi:10.1039/D3CE00871A

data_7247683
_publ_section_title
;
 Two isostructural complexes of Ni(ii) and Zn(ii) with violurate and
 pyridine: a detailed structural, theoretical, magnetic, and NMR
 investigation
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              6503
_journal_page_last               6511
_journal_paper_doi               10.1039/D3CE00871A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C22 H22 N8 O8 Zn, 3(H2 O)'
_chemical_formula_sum            'C22 H28 N8 O11 Zn'
_chemical_formula_weight         645.89
_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             2023-10-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-21 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                113.663(9)
_cell_angle_beta                 106.663(8)
_cell_angle_gamma                98.980(7)
_cell_formula_units_Z            2
_cell_length_a                   11.1064(9)
_cell_length_b                   12.1528(11)
_cell_length_c                   12.3032(12)
_cell_measurement_reflns_used    8428
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.462
_cell_measurement_theta_min      2.525
_cell_volume                     1385.8(3)
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_collection       'Bruker Apex 2'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Bruker Apex 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11499
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         33.851
_diffrn_reflns_theta_min         3.458
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         9459
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0589P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5823
_reflns_number_total             9459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00871a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7247682--7247683.cif.'
_cod_original_cell_volume        1385.8(2)
_cod_database_code               7247683
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.01
 H1WA-H1WB
 1.297 with sigma of 0.01
 O2W-H2WA = O2W-H2WB
 0.82 with sigma of 0.01
 H2WA-H2WB
 1.297 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(O11) = Uanis(O11A)
Uanis(O12) = Uanis(O12A)
Uanis(O13) = Uanis(O13A)
Uanis(O14) = Uanis(O14A)
Uanis(N11) = Uanis(N11A)
Uanis(N12) = Uanis(N12A)
Uanis(N13) = Uanis(N13A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C13) = Uanis(C13A)
Uanis(C14) = Uanis(C14A)
Uanis(C15) = Uanis(C15A)
Uanis(C16) = Uanis(C16A)
3. Same fragment restrains
{O11, O13, O14, N12, N13, C11, C12, C13, C14, C15, C16} sigma for 1-2: 0.02,
1-3: 0.04
as in
{O11A, O13A, O14A, N12A, N13A, C11A, C12A, C13A, C14A, C15A, C16A}
4. Others
 Sof(O12A)=Sof(N11A)=Sof(O11A)=Sof(O13A)=Sof(O14A)=Sof(N12A)=Sof(N13A)=
 Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(O12)=Sof(N11)=Sof(O11)=Sof(O13)=Sof(O14)=Sof(N12)=Sof(N13)=Sof(C11)=
 Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=
 Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(2)
 Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(2)
5.a Me refined with riding coordinates:
 C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F)
5.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C25(H25D,H25E,
 H25F), C26(H26A,H26B,H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57733
_shelx_fab_checksum              50043
_olex2_submission_special_instructions 'No special instructions were received'