Effect of ligand substitution on the SMM properties of three isostructural families of double-cubane Mn<sub>4</sub>Ln<sub>2</sub> coordination clusters.
Akhtar, Muhammad Nadeem; Lan, Yanhua; AlDamen, Murad A.; Zheng, Yan-Zhen; Anson, Christopher E.; Powell, Annie K.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3485–3495; doi:10.1039/c7dt04304j

data_7045402
_publ_section_title
;
 Effect of ligand substitution on the SMM properties of three
 isostructural families of double-cubane Mn<sub>4</sub>Ln<sub>2</sub>
 coordination clusters.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3485
_journal_page_last               3495
_journal_paper_doi               10.1039/c7dt04304j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C60 H116 Gd2 Mn4 N4 O26, 2.44(C2 H3 N), 0.56(H2 O)'
_chemical_formula_sum            'C64.88 H124.44 Gd2 Mn4 N6.44 O26.56'
_chemical_formula_weight         1954.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-12 deposited with the CCDC.
2018-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                64.935(1)
_cell_angle_beta                 66.609(1)
_cell_angle_gamma                80.602(1)
_cell_formula_units_Z            1
_cell_length_a                   13.1507(5)
_cell_length_b                   13.7341(5)
_cell_length_c                   13.8606(6)
_cell_measurement_reflns_used    10670
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.34
_cell_volume                     2081.25(14)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17392
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.033
_diffrn_reflns_theta_min         1.637
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    2.234
_exptl_absorpt_correction_T_max  0.676
_exptl_absorpt_correction_T_min  0.504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0380 before and 0.0218 after correction.
The Ratio of minimum to maximum transmission is 0.7456.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       block
_exptl_crystal_F_000             999
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.647
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8981
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0365P)^2^+7.8314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8295
_reflns_number_total             8981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04304j2.cif
_cod_data_source_block           21-mn4gd2
_cod_depositor_comments
'Adding full bibliography for 7045382--7045403.cif.'
_cod_original_cell_volume        2081.26(14)
_cod_database_code               7045402
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.574
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30B-C27 \\sim C30A-C27 \\sim C29C-C27 \\sim C29B-C27 \\sim C29A-C27 \\sim
C28C-C27 \\sim C28B-C27 ~
 C28A-C27 \\sim C30C-C27
 with sigma of 0.02
 C28A-C29A \\sim C29A-C30A \\sim C30A-C28A
 with sigma of 0.02
 C28B-C29B \\sim C29B-C30B \\sim C30B-C28B
 with sigma of 0.02
 C28C-C29C \\sim C29C-C30C \\sim C30C-C28C
 with sigma of 0.02
 N1B-C1B \\sim N1A-C1A \\sim N1B-C5B \\sim N1A-C5A \\sim N1A-C3 \\sim N1B-C3
 with sigma of 0.02
 C2B-C1B \\sim C2A-C1A
 with sigma of 0.02
 N2B-C7 \\sim N2A-C7 \\sim N2A-C2A \\sim N2B-C2B \\sim N2A-C9A \\sim N2B-C9B
 with sigma of 0.02
 C9A-C10A \\sim C9B-C10B
 with sigma of 0.02
 O5B-C10B \\sim O5A-C10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C22A \\sim C22B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006
C28B \\sim C28A \\sim C30C \\sim C30B \\sim C30A \\sim C29C \\sim C29B \\sim
C29A \\sim C28C \\sim C27: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C10B \\sim C10A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 C32, C31, N31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23A, C22A, C24A, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C21, C22B, C23B, C24B, C25B} sigma for 1-2: 0.02, 1-3: 0.04
as
{C21, C22A, C23A, C24A, C25A}
{C26, C27, C28B, C29B, C30B} sigma for 1-2: 0.02, 1-3: 0.04
{C26, C27, C28C, C29C, C30C} sigma for 1-2: 0.02, 1-3: 0.04
as
{C26, C27, C28A, C29A, C30A}
{N31, C31, C32} sigma for 1-2: 0.02, 1-3: 0.04
as
{N31B, C31B, C32B}
6. Others
 Fixed Sof: N1A(0.55) C1A(0.45) H1AA(0.45) H1AB(0.45) C2A(0.45) H2AA(0.45)
 H2AB(0.45) N2A(0.45) N1B(0.45) C1B(0.55) H1BA(0.55) H1BB(0.55) C2B(0.55)
 H2BA(0.55) H2BB(0.55) N2B(0.55) H3AA(0.55) H3AB(0.55) H3BC(0.45) H3BD(0.45)
 C5A(0.55) H5AA(0.55) H5AB(0.55) C6A(0.55) H6AA(0.55) H6AB(0.55) O3A(0.55)
 H3A(0.55) C5B(0.45) H5BA(0.45) H5BB(0.45) C6B(0.45) H6BA(0.45) H6BB(0.45)
 O3B(0.45) H3B(0.45) H7AA(0.45) H7AB(0.45) H7BC(0.55) H7BD(0.55) C9A(0.45)
 H9AA(0.45) H9AB(0.45) C10A(0.45) H10A(0.45) H10B(0.45) O5B(0.55) H5B(0.55)
 C9B(0.55) H9BA(0.55) H9BB(0.55) C10B(0.55) H10C(0.55) H10D(0.55) O5A(0.45)
 H5A(0.45) C22A(0.72) C23A(0.72) H23A(0.72) H23B(0.72) H23C(0.72) C24A(0.72)
 H24A(0.72) H24B(0.72) H24C(0.72) C25A(0.72) H25A(0.72) H25B(0.72) H25C(0.72)
 C22B(0.28) C23B(0.28) H23D(0.28) H23E(0.28) H23F(0.28) C24B(0.28) H24D(0.28)
 H24E(0.28) H24F(0.28) C25B(0.28) H25D(0.28) H25E(0.28) H25F(0.28) C28A(0.34)
 H28A(0.34) H28B(0.34) H28C(0.34) C29A(0.34) H29A(0.34) H29B(0.34) H29C(0.34)
 C30A(0.34) H30A(0.34) H30B(0.34) H30C(0.34) C28B(0.38) H28D(0.38) H28E(0.38)
 H28F(0.38) C29B(0.38) H29D(0.38) H29E(0.38) H29F(0.38) C30B(0.38) H30D(0.38)
 H30E(0.38) H30F(0.38) C28C(0.28) H28G(0.28) H28H(0.28) H28I(0.28) C29C(0.28)
 H29G(0.28) H29H(0.28) H29I(0.28) C30C(0.28) H30G(0.28) H30H(0.28) H30I(0.28)
 N31B(0.22) C31B(0.22) C32B(0.22) O31A(0.28)
7.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C2A(H2AA,H2AB), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C3(H3AA,H3AB),
  C3(H3BC,H3BD), C4(H4A,H4B), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C5B(H5BA,H5BB),
 C6B(H6BA,H6BB), C7(H7AA,H7AB), C7(H7BC,H7BD), C8(H8A,H8B), C9A(H9AA,H9AB),
 C10A(H10A,H10B), C9B(H9BA,H9BB), C10B(H10C,H10D)
7.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C),
 C25A(H25A,H25B,H25C), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F), C25B(H25D,
 H25E,H25F)
7.c Aromatic/amide H refined with riding coordinates:
 O3A(H3A), O3B(H3B), O5B(H5B), O5A(H5A)
7.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,
 H30B,H30C), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F),
 C28C(H28G,H28H,H28I), C29C(H29G,H29H,H29I), C30C(H30G,H30H,H30I), C32(H32A,
 H32B,H32C)
;
_shelx_res_checksum              16077
_olex2_submission_special_instructions 'No special instructions were received'