Elucidating the exchange interactions in a {GdIIICuII4} propellor
Heras Ojea, María José; Wilson, Claire; Cirera, Jordi; Oshio, Hiroki; Ruiz, Eliseo; Murrie, Mark; Dalton Transactions 52 (2023) 3203–3209; doi:10.1039/D2DT03901J

data_7712319
_publ_section_title
;
 Elucidating the exchange interactions in a {GdIIICuII4} propellor
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              3203
_journal_page_last               3209
_journal_paper_doi               10.1039/D2DT03901J
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety
'C44 H96 Cu4 Gd N8 O24, Cl O4, 6C H4 O), 2(Cl)'
_chemical_formula_sum            'C50 H120 Cl3 Cu4 Gd N8 O34'
_chemical_formula_weight         1895.29
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2020-03-06 deposited with the CCDC.	2023-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.610(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.405(2)
_cell_length_b                   11.0450(6)
_cell_length_c                   25.0948(17)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.43
_cell_volume                     7302.2(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1308
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48082
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.161
_diffrn_reflns_theta_max         25.161
_diffrn_reflns_theta_min         1.546
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.150
_exptl_absorpt_correction_T_max  0.9743
_exptl_absorpt_correction_T_min  0.7991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1268 before and 0.1058 after correction. The Ratio of minimum to maximum transmission is 0.8202. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3916
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.444
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         6489
_refine_ls_number_restraints     484
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0431P)^2^+24.8239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4688
_reflns_number_total             6489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03901j2.cif
_cod_data_source_block           1GdCu4
_cod_original_cell_volume        7302.0(8)
_cod_database_code               7712319
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{O4, O5}
3. Restrained distances
 O104-H104
 0.85 with sigma of 0.01
 O5-C5
 1.43 with sigma of 0.02
 C104-H104
 1.914597 with sigma of 0.02
 Cu1-H104
 3.173616 with sigma of 0.02
 Cl2-O4 \\sim Cl2-O1 \\sim Cl2-O3 \\sim Cl2-O2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O4) = Uanis(O5)
5. Rigid body (RIGU) restrains
 O106, Gd1, O209, O204, O105, O109, Cu1, Cu2, C209, C204, C105, C109, O104,
 N101, N102, N201, N202, C203, Cl1, C208, H20M, H20N, H20E, H20F, C103, H10G,
 H10H, C108, H10M, H10N, H201, C202, H104, C104, H101, C102, H102, C107, H202,
 C207, C205, C206, C210, C211, C106, C110, C111, C201, H20C, H20D, H10E, H10F,
 C101, H10C, H10D, H10K, H10L, H20K, H20L, O205, H20G, H20H, O206, H20I, H20J,
 O210, H21A, H21B, O211, H21C, H21D, H10I, H10J, O110, H11A, H11B, O111, H11C,
 H11D, H20A, H20B, H10A, H10B, H205, H206, H210, H211, H106, H110, H111, O2,
 Cl2, O1, O3, O4, O5, C5, C6, O6, H6, H6A, H6B, H6C, O8, H8, C8, H8A, H8B, H8C,
 O7, H7, C7, H7A, H7B, H7C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl2(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5) O6(0.5) H6(0.5) C6(0.5)
 H6A(0.5) H6B(0.5) H6C(0.5) O5(0.5) C5(0.5)
7.a Ternary CH refined with riding coordinates:
 N101(H101), N102(H102), N201(H201), N202(H202)
7.b Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C104(H10E,H10F), C105(H10G,H10H), C106(H10I,
 H10J), C107(H10K,H10L), C109(H10M,H10N), C110(H11A,H11B), C111(H11C,H11D),
 C201(H20A,H20B), C202(H20C,H20D), C204(H20E,H20F), C205(H20G,H20H), C206(H20I,
 H20J), C207(H20K,H20L), C209(H20M,H20N), C210(H21A,H21B), C211(H21C,H21D)
7.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
7.d Idealised tetrahedral OH refined as rotating group:
 O106(H106), O110(H110), O111(H111), O205(H205), O206(H206), O210(H210),
 O211(H211), O7(H7), O6(H6), O8(H8)
;
_shelx_res_checksum              78156
_shelx_hkl_checksum              13306
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'