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_7712321
_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 La N8 O24, 2(Cl), 2(C0.5 Cl0.5 O2.5), 3(C O), 2(C H4 O)'
_chemical_formula_sum            'C50 H120 Cl3 Cu4 La N8 O34'
_chemical_formula_weight         1876.95
_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             2016-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2020-03-06 deposited with the CCDC.	2023-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.674(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.5448(19)
_cell_length_b                   11.0401(3)
_cell_length_c                   25.2051(15)
_cell_measurement_reflns_used    6784
_cell_measurement_temperature    100(3)
_cell_measurement_theta_max      73.5590
_cell_measurement_theta_min      4.3250
_cell_volume                     7356.7(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42t (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42t (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42t (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2299
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -75.00  42.00   1.00    7.50    --  -38.50   0.00 120.00  117
  2  \w    -13.00  30.00   1.00    7.50    --  -38.50  38.00 -30.00   43
  3  \w     39.00  76.00   1.00    7.50    --   43.39-125.00  90.00   37
  4  \w     76.00 177.00   1.00   30.00    --  105.79  77.00  60.00  101
  5  \w     34.00 135.00   1.00   30.00    --  105.79 -77.00 -30.00  101
  6  \w     26.00 108.00   1.00   30.00    --  105.79 -94.00-180.00   82
  7  \w     36.00 118.00   1.00   30.00    --  105.79 -45.00 150.00   82
;
_diffrn_measurement_device_type  SuperNova
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11988
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.603
_exptl_absorpt_coefficient_mu    7.460
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42t (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       plate
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         6449
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0686P)^2^+2.2297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6141
_reflns_number_total             6449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03901j2.cif
_cod_data_source_block           4LaCu4
_cod_original_cell_volume        7356.7(9)
_cod_database_code               7712321
_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. Restrained distances
 O204-H204
 0.85 with sigma of 0.01
 O4-C7S
 1.43 with sigma of 0.02
 Cl2-O3 = Cl2-O1 = Cl2-O2 = Cl2-O4
 1.414 with sigma of 0.02
 C204-H204
 1.903621 with sigma of 0.02
 Cu2-H204
 3.150348 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O1, O2, O3, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O1, O2, O3, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O1SA)=1-FVAR(1)
 Sof(O1S)=FVAR(1)
 Fixed Sof: Cl2(0.5) O2(0.5) O3(0.5) O4(0.5) O5S(0.5) C6S(0.5) C7S(0.5)
5.a Ternary CH refined with riding coordinates:
 N31(H31), N35(H35), N101(H101), N102(H102)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C101(H10A,H10B), C102(H10C,H10D), C104(H10E,H10F), C105(H10G,
 H10H), C106(H10I,H10J), C107(H10K,H10L), C109(H10M,H10N), C110(H11A,H11B),
 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)
5.c Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC)
5.d Idealised tetrahedral OH refined as rotating group:
 O105(H105), O106(H106), O110(H110), O111(H111), O206(H206), O210(H210),
 O211(H211), O3S(H3S)
;
_shelx_res_checksum              9340
_shelx_hkl_checksum              70701
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-01-22
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;