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_7045397
_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 Pr2, 2(C2 H3 N), C7 H8, H2 O'
_chemical_formula_sum            'C71 H132 Mn4 N6 O27 Pr2'
_chemical_formula_weight         2003.40
_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             2018-01-10
_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                 92.650(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1710(7)
_cell_length_b                   14.5793(4)
_cell_length_c                   22.0369(6)
_cell_measurement_reflns_used    19781
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.41
_cell_volume                     8720.2(4)
_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(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29942
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.247
_diffrn_reflns_theta_min         1.818
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    1.733
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_correction_T_min  0.506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0400 before and 0.0201 after correction.
The Ratio of minimum to maximum transmission is 0.8573.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             4136
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         9868
_refine_ls_number_restraints     423
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+13.2495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9026
_reflns_number_total             9868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04304j2.cif
_cod_data_source_block           18-mn4pr2
_cod_depositor_comments
'Adding full bibliography for 7045382--7045403.cif.'
_cod_database_code               7045397
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.590
_shelx_estimated_absorpt_t_min   0.530
_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
 C12-C13A \\sim C12-C13B \\sim C12-C13C \\sim C12-C14A \\sim C12-C14B \\sim
C12-C14C \\sim C12-C15A ~
 C12-C15B \\sim C12-C15C
 with sigma of 0.02
 C13A-C14A \\sim C14A-C15A \\sim C15A-C13A
 with sigma of 0.02
 C13B-C14B \\sim C14B-C15B \\sim C15B-C13B
 with sigma of 0.02
 C13C-C14C \\sim C14C-C15C \\sim C15C-C13C
 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
3. Uiso/Uaniso restraints and constraints
Uanis(C32A) = Uanis(C32B)
4. Rigid body (RIGU) restrains
 C41, C42, C43, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N31B, C31B, C32B, C32A, C31A, N31A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, N1A, N1B, C1A, C2A, C1B, C2B, N2A, N2B, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C23, C22B, C22A, C24A, C24B, C25A, C25B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Mn2, O3A, O3B, C6B, C6A, C5B, C5A, N1A, N1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2A, N2B, C9A, C9B, C10A, C10B, O5B, O5A, Mn2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27B, C30B, C28B, C29B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27A, C30A, C29A, C28A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C21, C22B, C23, C24B, C25B} sigma for 1-2: 0.02, 1-3: 0.04
as
{C21, C22A, C23, C24A, C25A}
{C26, C27B, C28B, C29B, C30B} sigma for 1-2: 0.02, 1-3: 0.04
as
{C26, C27A, C28A, C29A, C30A}
{N31B, C31B, C32B} sigma for 1-2: 0.02, 1-3: 0.04
as
{N31A, C31A, C32A}
6. Others
 Fixed Sof: N1A(0.55) C1A(0.55) H1AA(0.55) H1AB(0.55) C2A(0.55) H2AA(0.55)
 H2AB(0.55) N2A(0.55) N1B(0.45) C1B(0.45) H1BA(0.45) H1BB(0.45) C2B(0.45)
 H2BA(0.45) H2BB(0.45) N2B(0.45) 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(0.55) H7AB(0.55) H7BC(0.45) H7BD(0.45) C9A(0.55)
 H9AA(0.55) H9AB(0.55) C10A(0.55) H10A(0.55) H10B(0.55) O5A(0.55) H5A(0.55)
 C9B(0.45) H9BA(0.45) H9BB(0.45) C10B(0.45) H10C(0.45) H10D(0.45) O5B(0.45)
 H5B(0.45) C13A(0.48) H13A(0.48) H13B(0.48) H13C(0.48) C14A(0.48) H14A(0.48)
 H14B(0.48) H14C(0.48) C15A(0.48) H15A(0.48) H15B(0.48) H15C(0.48) C14B(0.22)
 H14D(0.22) H14E(0.22) H14F(0.22) C13B(0.22) H13D(0.22) H13E(0.22) H13F(0.22)
 C15B(0.22) H15D(0.22) H15E(0.22) H15F(0.22) C13C(0.3) H13G(0.3) H13H(0.3)
 H13I(0.3) C14C(0.3) H14G(0.3) H14H(0.3) H14I(0.3) C15C(0.3) H15G(0.3)
 H15H(0.3) H15I(0.3) C22A(0.44) H23A(0.44) H23B(0.44) H23C(0.44) H23D(0.56)
 H23E(0.56) H23F(0.56) C24A(0.44) H24A(0.44) H24B(0.44) H24C(0.44) C25A(0.44)
 H25A(0.44) H25B(0.44) H25C(0.44) C22B(0.56) C24B(0.56) H24D(0.56) H24E(0.56)
 H24F(0.56) C25B(0.56) H25D(0.56) H25E(0.56) H25F(0.56) C27A(0.5) C28A(0.5)
 H28A(0.5) H28B(0.5) H28C(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) C28B(0.5) H28D(0.5)
 H28E(0.5) H28F(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(0.58) C31A(0.58) C32A(0.58) H32A(0.58)
 H32B(0.58) H32C(0.58) N31B(0.42) C31B(0.42) C32B(0.42) H32D(0.42) H32E(0.42)
 H32F(0.42) C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5)
 H44(0.5) C45(0.5) H45(0.5) C46(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5)
 O51B(0.5)
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:
 C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C14B(H14D,
 H14E,H14F), C13B(H13D,H13E,H13F), C15B(H15D,H15E,H15F), C13C(H13G,H13H,H13I),
 C14C(H14G,H14H,H14I), C15C(H15G,H15H,H15I), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C23(H23D,H23E,H23F),
 C24A(H24A,H24B,H24C), C25A(H25A,H25B,H25C), C24B(H24D,H24E,H24F), C25B(H25D,
 H25E,H25F), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C),
 C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F)
7.c Aromatic/amide H refined with riding coordinates:
 O3A(H3A), O3B(H3B), O5A(H5A), O5B(H5B), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45)
7.d Fitted hexagon refined as free rotating group:
 C41(C42,C43,C44,C45,C46)
7.e Idealised Me refined as rotating group:
 C32A(H32A,H32B,H32C), C32B(H32D,H32E,H32F), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              80871
_olex2_submission_special_instructions 'No special instructions were received'