Synthesis, structural features, magnetic properties and thermal decomposition of a new series of polymeric Ln(iii)–Cr(iii) cyclopropane-1,1-dicarboxylates
Bazhina, Evgeniya S.; Shmelev, Maxim A.; Voronina, Julia K.; Korotkova, Natalia A.; Babeshkin, Konstantin A.; Matiukhina, Anna K.; Belova, Ekaterina V.; Gogoleva, Natalia V.; Kottsov, Sergey Yu.; Efimov, Nikolay N.; Kiskin, Mikhail A.; Eremenko, Igor L.; New Journal of Chemistry 47 (2023) 19251–19264; doi:10.1039/D3NJ03027J

data_7062793
_publ_section_title
;
 Synthesis, structural features, magnetic properties and thermal
 decomposition of a new series of polymeric Ln(iii)--Cr(iii)
 cyclopropane-1,1-dicarboxylates
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19251
_journal_page_last               19264
_journal_paper_doi               10.1039/D3NJ03027J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C30 H42 Cr2 O33 Tb2, 17(H O0.5)'
_chemical_formula_sum            'C30 H59 Cr2 O41.5 Tb2'
_chemical_formula_weight         1505.61
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-12-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-23 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2441(3)
_cell_length_b                   16.2441(3)
_cell_length_c                   38.4605(17)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      30.11
_cell_measurement_theta_min      2.39
_cell_volume                     10148.6(5)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            84053
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.850
_exptl_absorpt_coefficient_mu    3.286
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0767 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.8771.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_description       plate
_exptl_crystal_F_000             5992
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 3881 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         9976
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      2.824
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0235P)^2^+13.6214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9384
_reflns_number_total             9976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03027j2.cif
_cod_data_source_block           a_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7062789--7062793.cif.'
_cod_original_cell_volume        10148.6(6)
_cod_original_formula_sum        'C30 H59 Cr2 O41.50 Tb2'
_cod_database_code               7062793
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H4A-H1S
 2.1 with sigma of 0.02
 H4SA-H4B
 2.6 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O4S) \\sim Ueq, Uanis(O4S') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O4S') = Uanis(O4S)
Uanis(O7S) = Uanis(O7')
Uanis(O6S) = Uanis(O8S)
Uanis(O8') = Uanis(O8S)
4. Others
 Sof(O7')=Sof(H7'A)=Sof(H7'B)=1-FVAR(1)
 Sof(O7S)=Sof(H7SA)=Sof(H7SB)=FVAR(1)
 Sof(O9')=Sof(H9'A)=Sof(H9'B)=1-FVAR(2)
 Sof(O9S)=Sof(H9SA)=Sof(H9SB)=FVAR(2)
 Sof(O8')=Sof(H8'A)=Sof(H8'B)=1-FVAR(3)
 Sof(O8S)=Sof(H8SA)=Sof(H8SB)=FVAR(3)
 Sof(O4S')=Sof(H4SC)=Sof(H4SD)=1-FVAR(4)
 Sof(O4S)=Sof(H4SA)=Sof(H4SB)=FVAR(4)
5.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B),
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O1S(H1S), O2S(H2SA,H2SB), O3S(H3SA,
 H3SB), O4S(H4SA,H4SB), O5S(H5SA,H5SB), O4S'(H4SC,H4SD), O6S(H6SA,H6SB),
 O7S(H7SA,H7SB), O8S(H8SA,H8SB), O7'(H7'A,H7'B), O8'(H8'A,H8'B), O9S(H9SA,H9SB),
  O9'(H9'A,H9'B)
5.b Secondary CH2 refined with riding coordinates:
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C14A(H14A,
 H14B), C15A(H15A,H15B), C4B(H4BA,H4BB), C5B(H5BA,H5BB), C9B(H9BA,H9BB),
 C10B(H10C,H10D), C14B(H14C,H14D), C15B(H15C,H15D)
;
_shelx_res_checksum              52959
_olex2_submission_special_instructions 'No special instructions were received'