Nickel(ii)-mediated in situ complex formation with unexpected ligand transformations: crystal structures, DFT calculations, and catalytic activity in CO2 fixation reactions
Dolai, Malay; Saha, Urmila; Goswami, Juli Nanda; Bhattacharya, Biswajit; Emmerling, Franziska; Ifseisi, Ahmad A.; Biswas, Surajit; New Journal of Chemistry 49 (2025) 4451–4463; doi:10.1039/D4NJ01801J

data_7063660
_publ_section_title
;
 Nickel(ii)-mediated in situ complex formation with unexpected ligand
 transformations: crystal structures, DFT calculations, and catalytic
 activity in CO2 fixation reactions
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4451
_journal_page_last               4463
_journal_paper_doi               10.1039/D4NJ01801J
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety
'C32 H30 Cl2 N18 Ni2 O4, 2(Cl), 5.563(H2 O), 1.437(C H4 O)'
_chemical_formula_sum            'C33.44 H46.88 Cl4 N18 Ni2 O11'
_chemical_formula_weight         1136.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-21 deposited with the CCDC.	2025-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.013(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.354(3)
_cell_length_b                   10.5144(13)
_cell_length_c                   21.722(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.776
_cell_measurement_theta_min      2.170
_cell_volume                     4751.9(11)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30906
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.776
_diffrn_reflns_theta_min         2.283
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Multi-scan
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       Rodlike
_exptl_crystal_F_000             2342
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5012
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0646P)^2^+5.6572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4183
_reflns_number_total             5012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01801j2.cif
_cod_data_source_block           bb232
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7063659--7063660.cif.
;
_cod_original_cell_volume        4751.7(10)
_cod_database_code               7063660
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7A-C18 = O5-C17
 1.43 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O7) = Uanis(C18)
Uanis(O7A) = Uanis(O7)
4. Others
 Sof(Cl3)=1-FVAR(1)
 Sof(Cl2)=FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O7A)=Sof(H7A)=1-FVAR(2)
 Sof(O7)=Sof(H7B)=Sof(H7C)=FVAR(2)
 Fixed Sof: C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) O5(0.5) H5(0.5)
5.a Free rotating group:
 O6(H6A,H6B), O3(H3A,H3B), O7(H7B,H7C)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C2(H2), C9(H9), C3(H3), C13(H13), C10(H10), C15(H15), C14(H14)
5.c X=CH2 refined with riding coordinates:
 N5(H5A,H5B)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
5.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O7A(H7A)
;
_olex2_submission_special_instructions 'No special instructions were received'