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_7045395
_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 Mn4 N4 O26 Tb2, 2(C2 H3 N), C7 H8, H2 O'
_chemical_formula_sum            'C71 H132 Mn4 N6 O27 Tb2'
_chemical_formula_weight         2039.42
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90
_cell_angle_beta                 92.776(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.154(2)
_cell_length_b                   14.4968(13)
_cell_length_c                   21.8243(19)
_cell_measurement_reflns_used    19732
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.43
_cell_volume                     8581.0(12)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2000)'
_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    'SHELXS (Sheldrick, 2003)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.924
_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  0.0197
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27332
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.195
_diffrn_reflns_theta_min         1.868
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.577
_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 0.0207 after correction.
The Ratio of minimum to maximum transmission is 0.8103.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             4184
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.275
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         9762
_refine_ls_number_restraints     392
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+33.9966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9053
_reflns_number_total             9762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04304j2.cif
_cod_data_source_block           22-mn4tb2
_cod_depositor_comments
'Adding full bibliography for 7045382--7045403.cif.'
_cod_original_cell_volume        8581.1(13)
_cod_database_code               7045395
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.569
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, 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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C25A-C22A \\sim C24A-C22A \\sim C23A-C22A
 with sigma of 0.02
 C23B-C22B \\sim C24B-C22B \\sim C25B-C22B
 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
 O5A-C10A \\sim O5B-C10B
 with sigma of 0.02
 C2A-C1A \\sim C2B-C1B
 with sigma of 0.02
 N1A-C3 \\sim N1B-C3 \\sim N1B-C1B \\sim N1A-C1A \\sim N1B-C5B \\sim N1A-C5A
\\sim C6B-C5B \\sim C6A-C5A
 with sigma of 0.02
 O3B-C6B \\sim O3A-C6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C32A) = Uanis(C32B)
4. Rigid body (RIGU) restrains
 C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22A, C22B, C25B, C23A, C23B, C25A, C24B, C24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18A, C17, C20A, C19A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N31B, C31B, C32B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N31A, C31A, C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3B, O3A, Mn2, C6A, C6B, C5A, C5B, N1A, N1B, C3, C1A, C1B, C2A, C2B, N2A, N2B,
  C7, C9A, C10A, C10B, O5B, O5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1A(0.47) C1A(0.47) H1AA(0.47) H1AB(0.47) C2A(0.47) H2AA(0.47)
 H2AB(0.47) N2A(0.47) N1B(0.53) C1B(0.53) H1BA(0.53) H1BB(0.53) C2B(0.53)
 H2BA(0.53) H2BB(0.53) N2B(0.53) H3AA(0.47) H3AB(0.47) H3BC(0.53) H3BD(0.53)
 C5A(0.47) H5AA(0.47) H5AB(0.47) C6A(0.47) H6AA(0.47) H6AB(0.47) O3A(0.47)
 H3A(0.47) C5B(0.53) H5BA(0.53) H5BB(0.53) C6B(0.53) H6BA(0.53) H6BB(0.53)
 O3B(0.53) H3B(0.53) H7AA(0.47) H7AB(0.47) H7BC(0.53) H7BD(0.53) C9A(0.47)
 H9AA(0.47) H9AB(0.47) C10A(0.47) H10A(0.47) H10B(0.47) O5A(0.47) H5A(0.47)
 C9B(0.53) H9BA(0.53) H9BB(0.53) C10B(0.53) H10C(0.53) H10D(0.53) O5B(0.53)
 H5B(0.53) C18A(0.62) H18A(0.62) H18B(0.62) H18C(0.62) C19A(0.62) H19A(0.62)
 H19B(0.62) H19C(0.62) C20A(0.62) H20A(0.62) H20B(0.62) H20C(0.62) C18B(0.38)
 H18D(0.38) H18E(0.38) H18F(0.38) C19B(0.38) H19D(0.38) H19E(0.38) H19F(0.38)
 C20B(0.38) H20D(0.38) H20E(0.38) H20F(0.38) C22A(0.5) C23A(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5) C24A(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25A(0.5)
 H25A(0.5) H25B(0.5) H25C(0.5) C22B(0.5) C23B(0.5) H23D(0.5) H23E(0.5)
 H23F(0.5) C24B(0.5) H24D(0.5) H24E(0.5) H24F(0.5) C25B(0.5) H25D(0.5)
 H25E(0.5) H25F(0.5) C27A(0.5) H28A(0.5) H28B(0.5) H28C(0.5) H28D(0.5)
 H28E(0.5) H28F(0.5) C29A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30A(0.5)
 H30A(0.5) H30B(0.5) H30C(0.5) C27B(0.5) C29B(0.5) H29D(0.5) H29E(0.5)
 H29F(0.5) C30B(0.5) H30D(0.5) H30E(0.5) H30F(0.5) N31A(0.5) C31A(0.5)
 C32A(0.5) H32A(0.5) H32B(0.5) H32C(0.5) N31B(0.5) C31B(0.5) C32B(0.5)
 H32D(0.5) H32E(0.5) H32F(0.5) H42(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5)
 O51B(0.5)
6.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)
6.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18A(H18A,H18B,
 H18C), C19A(H19A,H19B,H19C), C20A(H20A,H20B,H20C), C18B(H18D,H18E,H18F),
 C19B(H19D,H19E,H19F), C20B(H20D,H20E,H20F), C23A(H23A,H23B,H23C), C24A(H24A,
 H24B,H24C), C25A(H25A,H25B,H25C), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F),
 C25B(H25D,H25E,H25F), C28(H28A,H28B,H28C), C28(H28D,H28E,H28F), C29A(H29A,H29B,
 H29C), C30A(H30A,H30B,H30C), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F),
 C45(H45A,H45B,H45C)
6.c Aromatic/amide H refined with riding coordinates:
 O3A(H3A), O3B(H3B), O5A(H5A), O5B(H5B), C41(H41), C42(H42), C43(H43), C44(H44)
6.d Idealised Me refined as rotating group:
 C32A(H32A,H32B,H32C), C32B(H32D,H32E,H32F)
;
_shelx_res_checksum              16061
_olex2_submission_special_instructions 'No special instructions were received'