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_7045394
_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
'C60.6 H117.8 Mn4 N4 Nd2 O26, 2(C2 H3 N), C7 H8, H2 O'
_chemical_formula_sum            'C71 H132 Mn4 N6 Nd2 O27'
_chemical_formula_weight         2010.06
_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   mixed
_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                 92.649(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1777(17)
_cell_length_b                   14.5314(9)
_cell_length_c                   21.9879(14)
_cell_measurement_reflns_used    8199
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.33
_cell_volume                     8674.4(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.913
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23539
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.197
_diffrn_reflns_theta_min         1.589
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    1.816
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0347 before and 0.0260 after correction.
The Ratio of minimum to maximum transmission is 0.8398.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         9762
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0383P)^2^+8.0020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8395
_reflns_number_total             9762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04304j2.cif
_cod_data_source_block           19-mn4nd2
_cod_depositor_comments
'Adding full bibliography for 7045382--7045403.cif.'
_cod_database_code               7045394
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.594
_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
 C46-C47
 1.5 with sigma of 0.02
 O3A-H3A = O3B-H3B = O5B-H5B = O5A-H5A
 0.88 with sigma of 0.04
 H5A-O12 = H5B-O12
 1.89 with sigma of 0.04
 C12-C13A \\sim C12-C14A \\sim C12-C15A \\sim C12-C13B \\sim C12-C14B \\sim
C12-C15B \\sim C12-C13C ~
 C12-C14C \\sim C12-C15C
 with sigma of 0.02
 C13A-C14A \\sim C14A-C15A \\sim C15A-C13A \\sim C13B-C14B \\sim C14B-C15B
\\sim C15B-C13B \\sim C13C-
 C14C \\sim C14C-C15C \\sim C15C-C13C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C32A \\sim C32B: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006
C12 \\sim C13A \\sim C14A \\sim C15A \\sim C13B \\sim C14B \\sim C15B \\sim
C13C \\sim C14C \\sim C15C: within 2A with sigma of 0.006 and sigma for
terminal atoms of 0.012
4. Rigid body (RIGU) restrains
 C26, C27A, C28A, C29A, C30A, C27B, C28B, C29B, C30B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 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
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(0.47) H13A(0.47) H13B(0.47) H13C(0.47) C14A(0.47) H14A(0.47)
 H14B(0.47) H14C(0.47) C15A(0.47) H15A(0.47) H15B(0.47) H15C(0.47) C13B(0.22)
 H13D(0.22) H13E(0.22) H13F(0.22) C14B(0.22) H14D(0.22) H14E(0.22) H14F(0.22)
 C15B(0.22) H15D(0.22) H15E(0.22) H15F(0.22) C13C(0.41) H13G(0.41) H13H(0.41)
 H13I(0.41) C14C(0.41) H14G(0.41) H14H(0.41) H14I(0.41) C15C(0.41) H15G(0.41)
 H15H(0.41) H15I(0.41) C22A(0.45) H23A(0.45) H23B(0.45) H23C(0.45) H23D(0.55)
 H23E(0.55) H23F(0.55) C24A(0.45) H24A(0.45) H24B(0.45) H24C(0.45) C25A(0.45)
 H25A(0.45) H25B(0.45) H25C(0.45) C22B(0.55) C24B(0.55) H24D(0.55) H24E(0.55)
 H24F(0.55) C25B(0.55) H25D(0.55) H25E(0.55) H25F(0.55) 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(0.55) C31A(0.55) C32A(0.55) H32A(0.55)
 H32B(0.55) H32C(0.55) N31B(0.45) C31B(0.45) C32B(0.45) H32D(0.45) H32E(0.45)
 H32F(0.45) 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), C13B(H13D,
 H13E,H13F), C14B(H14D,H14E,H14F), 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:
 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              81727
_olex2_submission_special_instructions 'No special instructions were received'