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_7712322
_publ_section_title
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 Elucidating the exchange interactions in a {GdIIICuII4} propellor
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_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 Dy N8 O24, 2(Cl), Cl O4, 6(C H4 O)'
_chemical_formula_sum            'C50 H120 Cl3 Cu4 Dy N8 O34'
_chemical_formula_weight         1900.54
_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             2020-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-06 deposited with the CCDC.	2023-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.646(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.254(4)
_cell_length_b                   11.0373(12)
_cell_length_c                   25.039(3)
_cell_measurement_reflns_used    9766
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.67
_cell_volume                     7243.7(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40409
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.248
_diffrn_reflns_theta_min         2.000
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.283
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1117 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.9130.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       Tablet
_exptl_crystal_F_000             3924
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.560
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         8960
_refine_ls_number_restraints     418
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+68.7297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8089
_reflns_number_total             8960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03901j2.cif
_cod_data_source_block           3DyCu4
_cod_original_cell_volume        7243.6(15)
_cod_database_code               7712322
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,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
 O5-C5
 1.43 with sigma of 0.02
 O106-C106
 1.43 with sigma of 0.02
 O104-H104
 0.85 with sigma of 0.01
 O11B-C110 = O110-C110
 1.43 with sigma of 0.02
 C104-H104
 1.914362 with sigma of 0.02
 Cu1-H104
 3.184872 with sigma of 0.02
 Cl2-O4 \\sim Cl2-O1 \\sim Cl2-O3 \\sim Cl2-O2
 with sigma of 0.02
 O11B-C110 \\sim O110-C110
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O4) = Uanis(O5)
5. Rigid body (RIGU) restrains
 Dy1, Cu1, Cu2, O104, O105, O106, O109, O110, O111, O204, O205, O206, O209,
 O210, O211, N101, N102, N201, N202, C101, C102, C103, C104, C105, C106, C107,
 C108, C109, C110, C111, C201, C202, C203, C204, C205, C206, C207, C208, C209,
 C210, C211, Cl1, Cl2, O1, O2, O3, O4, O8, C8, O6, C6, O7, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O11B)=Sof(H11B)=Sof(H11D)=Sof(H11E)=1-FVAR(1)
 Sof(O110)=Sof(H110)=Sof(H11A)=Sof(H11C)=FVAR(1)
 Fixed Sof: Cl2(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5) O5(0.5) C5(0.5) O1AA(0.2)
 O2AA(0.15) O8(0.65) O6(0.5) C6(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(H11D,H11E), C110(H11A,H11C),
 C111(H11F,H11G), 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 Tetrahedral OH refined with riding coordinates:
 O11B(H11B)
7.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
7.e Idealised tetrahedral OH refined as rotating group:
 O106(H106), O110(H110), O111(H111), O205(H205), O206(H206), O210(H210),
 O211(H211), O7(H7)
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_shelx_res_checksum              64227
_shelx_hkl_checksum              85462
_olex2_submission_special_instructions 'No special instructions were received'