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_7250200
_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 Ni3 O38 Rb6, 3.5[H2O]'
_chemical_formula_sum            'C30 H59 Ni3 O41.5 Rb6'
_chemical_formula_weight         1772.72
_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             2025-02-03
_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                78.142(2)
_cell_angle_beta                 66.982(2)
_cell_angle_gamma                78.702(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5074(11)
_cell_length_b                   12.4178(13)
_cell_length_c                   12.4907(13)
_cell_measurement_reflns_used    787
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     1455.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector''
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26265
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.647
_diffrn_reflns_theta_min         1.690
_exptl_absorpt_coefficient_mu    6.047
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_description       block
_exptl_crystal_F_000             877
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         8965
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.4581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7751
_reflns_number_total             8965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01319k2.cif
_cod_data_source_block           96_2
_cod_depositor_comments
'Adding full bibliography for 7250200--7250203.cif.'
_cod_original_formula_sum        'C30 H59 Ni3 O41.50 Rb6'
_cod_database_code               7250200
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.507
_shelx_estimated_absorpt_t_min   0.363
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O4W-H4WA
 0.87 with sigma of 0.002
 O7W-H7WB
 0.87 with sigma of 0.002
 H6WB-O6W
 0.87 with sigma of 0.002
 H5WB-O5W
 0.87 with sigma of 0.002
 O7W-H7WA
 0.87 with sigma of 0.002
 O4W-H4WB
 0.87 with sigma of 0.002
 O6W-H6WA
 0.87 with sigma of 0.002
 O5W-H5WA
 0.87 with sigma of 0.002
3.a Free rotating group:
 H1WA(H1WB), H2WA(H2WB), H3WA(H3WB), H4WA(H4WB), H5WA(H5WB), H6WA(H6WB),
 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)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 35 electrons were 
found in a volume of 94\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3.5[H2O] per formula unit 
which account for 35 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47598
_shelx_fab_checksum              83340
_olex2_submission_special_instructions 'No special instructions were received'