The role of alkali metal cations in the construction of heterometallic NiII polymeric cyclopropane-1,1-dicarboxylates
Zorina-Tikhonova, Ekaterina N.; Matiukhina, Anna K.; Korlyukov, Alexander A.; Goloveshkin, Alexander S.; Babeshkin, Konstantin A.; Efimov, Nikolay N.; Alexandrov, Eugeny V.; Kiskin, Mikhail A.; Eremenko, Igor L.; CrystEngComm 27 (2025) 3352–3361; doi:10.1039/D4CE01319K

data_7250203
_publ_section_title
;
 The role of alkali metal cations in the construction of heterometallic
 NiII polymeric cyclopropane-1,1-dicarboxylates
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              3352
_journal_page_last               3361
_journal_paper_doi               10.1039/D4CE01319K
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C30 H52 K6 Ni3 O38, 4(H2 O)'
_chemical_formula_sum            'C30 H60 K6 Ni3 O42'
_chemical_formula_weight         1503.51
_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             2025-02-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-21 deposited with the CCDC.	2025-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                75.425(3)
_cell_angle_beta                 66.665(2)
_cell_angle_gamma                78.791(3)
_cell_formula_units_Z            1
_cell_length_a                   10.2896(18)
_cell_length_b                   12.302(2)
_cell_length_c                   12.719(2)
_cell_measurement_reflns_used    4070
_cell_measurement_temperature    184(2)
_cell_measurement_theta_max      30.71
_cell_measurement_theta_min      2.25
_cell_volume                     1422.6(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      184.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14737
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.720
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0778 before and 0.0394 after correction.
The Ratio of minimum to maximum transmission is 0.7380.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7002
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      85.356
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0363P)^2^+1.9716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5520
_reflns_number_total             7002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01319k2.cif
_cod_data_source_block           nip
_cod_depositor_comments
'Adding full bibliography for 7250200--7250203.cif.'
_cod_original_cell_volume        1422.5(4)
_cod_database_code               7250203
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.730
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All O(H,H,H,H,H,H) groups
2. Restrained distances
 O1W-H1WB = O1W-H1WA
 0.82 with sigma of 0.01
 H7WB-O6W
 2.939 with sigma of 0.002
 H6WA-O6W
 0.88 with sigma of 0.002
 O9W-H9WA = O9W-H9WB
 0.82 with sigma of 0.01
 H7WB-O7W
 0.88 with sigma of 0.002
 H9WA-H9WB
 1.33 with sigma of 0.02
 O7W-H7WA
 0.88 with sigma of 0.002
 O8W-H8WB = O8W-H8WA
 0.82 with sigma of 0.01
 H7WA-O2_$4
 1.95 with sigma of 0.002
 H1WB-H1WA
 1.33 with sigma of 0.02
 H7WB-O8W_$3
 2.03 with sigma of 0.002
 O2W-H2WA = O2W-H2WB
 0.82 with sigma of 0.01
 H2WA-H2WB
 1.33 with sigma of 0.02
 O3W-H3WA = O3W-H3WB
 0.82 with sigma of 0.01
 H3WA-H3WB
 1.33 with sigma of 0.02
 O4W-H4WA = O4W-H4WB
 0.82 with sigma of 0.01
 H4WA-H4WB
 1.33 with sigma of 0.02
 O5W-H5WA = O5W-H5WB
 0.82 with sigma of 0.01
 H5WA-H5WB
 1.33 with sigma of 0.02
 H8WB-H8WA
 1.33 with sigma of 0.02
 H7WB-H7WA
 1.359 with sigma of 0.002
3.a Free rotating group:
 H7WA(H7WB)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C9(H9A,H9B), C10(H10A,H10B), C14(H14A,H14B),
 C15(H15A,H15B)
;
_shelx_res_checksum              83922
_olex2_submission_special_instructions 'No special instructions were received'