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_7247682
_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 Ni O8, 3(H2 O)'
_chemical_formula_sum            'C22 H28 N8 Ni O11'
_chemical_formula_weight         639.23
_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                112.946(5)
_cell_angle_beta                 106.988(4)
_cell_angle_gamma                99.066(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9490(5)
_cell_length_b                   11.9806(7)
_cell_length_c                   12.0973(6)
_cell_measurement_reflns_used    9336
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.877
_cell_measurement_theta_min      2.437
_cell_volume                     1329.49(15)
_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    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker Apex 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7951
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.625
_diffrn_reflns_theta_min         4.439
_exptl_absorpt_coefficient_mu    1.728
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            green-blue
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         5070
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0388P)^2^+0.6029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4486
_reflns_number_total             5070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00871a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7247682--7247683.cif.'
_cod_original_cell_volume        1329.48(13)
_cod_database_code               7247682
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Restrained distances
 O1W-H1WA = O1W-H1WB = O2W-H2WA = O2W-H2WB = O3WA-H3WA
 0.85 with sigma of 0.01
 H1WA-H1WB = H2WA-H2WB
 1.34 with sigma of 0.01
 N21-C21 \\sim N21-C23 \\sim N21A-C21A \\sim N21A-C23A
 with sigma of 0.01
 N21-O22 \\sim N21A-O22A
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
O3WA \\sim O3WB \\sim O3WC: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.005 within 2A
Uanis(O21) = Uanis(O21A)
Uanis(O22) = Uanis(O22A)
Uanis(O23) = Uanis(O23A)
Uanis(O24) = Uanis(O24A)
Uanis(N21) = Uanis(N21A)
Uanis(N22) = Uanis(N22A)
Uanis(N23) = Uanis(N23A)
Uanis(C21) = Uanis(C21A)
Uanis(C22) = Uanis(C22A)
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
3. Same fragment restrains
{O21, O23, O24, N22, N23, C21, C22, C23, C24, C25, C26} sigma for 1-2: 0.02,
1-3: 0.04
as in
{O21A, O23A, O24A, N22A, N23A, C21A, C22A, C23A, C24A, C25A, C26A}
4. Others
 Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(O21A)=Sof(O23A)=Sof(O24A)=Sof(N22A)=Sof(N23A)=Sof(C21A)=Sof(C22A)=
 Sof(C23A)=Sof(C24A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=
 Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(O22A)=Sof(N21A)=1-FVAR(2)
 Sof(O21)=Sof(O23)=Sof(O24)=Sof(N22)=Sof(N23)=Sof(C21)=Sof(C22)=Sof(C23)=
 Sof(C24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(O22)=Sof(N21)=FVAR(2)
 Fixed Sof: O3WA(0.5) H3WA(0.5) O3WB(0.1) O3WC(0.15)
5.a Me refined with riding coordinates:
 C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F)
5.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C15(H15D,H15E,H15F), C16(H16A,H16B,H16C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              33351
_olex2_submission_special_instructions 'No special instructions were received'