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_7045389
_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         'C50 H98 Er2 Mn4 N6 O28, 3(C2 H3 N)'
_chemical_formula_sum            'C56 H107 Er2 Mn4 N9 O28'
_chemical_formula_weight         1908.78
_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             2018-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
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2018-01-12 deposited with the CCDC.
2018-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.852(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.901(3)
_cell_length_b                   13.9253(11)
_cell_length_c                   22.556(3)
_cell_measurement_reflns_used    8002
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.02
_cell_volume                     7593.9(16)
_computing_cell_refinement       'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_data_collection       'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_data_reduction        'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_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      220(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24444
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.959
_diffrn_reflns_theta_min         2.022
_exptl_absorpt_coefficient_mu    2.912
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             3864
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.789
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7110
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+9.8722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5922
_reflns_number_total             7110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04304j2.cif
_cod_data_source_block           10-mn4er2
_cod_depositor_comments
'Adding full bibliography for 7045382--7045403.cif.'
_cod_original_cell_volume        7594.0(15)
_cod_database_code               7045389
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.530
_shelx_estimated_absorpt_t_min   0.447
_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
 O3A-H3AA = O3B-H3AA = O5-H5
 0.88 with sigma of 0.02
 C6B-C5 \\sim C6A-C5
 with sigma of 0.02
 O3B-C6B \\sim O3A-C6A
 with sigma of 0.02
 N31A-C31A \\sim N31B-C31B \\sim N32-C33
 with sigma of 0.02
 C32B-C31B \\sim C32A-C31A \\sim C34-C33
 with sigma of 0.02
 N31A-C32A \\sim N31B-C32B \\sim N32-C34
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O3A, O3B, C6A, C6B, C5, Mn2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C16, C17, C18B, C19B, C20B} sigma for 1-2: 0.02, 1-3: 0.04
as
{C16, C17, C18A, C19A, C20A}
5. Others
 Fixed Sof: H5AA(0.59) H5AB(0.59) H5BC(0.41) H5BD(0.41) C6A(0.59) H6AA(0.59)
 H6AB(0.59) O3A(0.59) C6B(0.41) H6BA(0.41) H6BB(0.41) O3B(0.41) C18A(0.51)
 H18A(0.51) H18B(0.51) H18C(0.51) C19A(0.51) H19A(0.51) H19B(0.51) H19C(0.51)
 C20A(0.51) H20A(0.51) H20B(0.51) H20C(0.51) C18B(0.49) H18D(0.49) H18E(0.49)
 H18F(0.49) C19B(0.49) H19D(0.49) H19E(0.49) H19F(0.49) C20B(0.49) H20D(0.49)
 H20E(0.49) H20F(0.49) H34A(0.5) H34B(0.5) H34C(0.5) C31A(0.5) N31B(0.5)
 N31A(0.5) C32B(0.5) C31B(0.5) C32A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5AA,H5AB), C5(H5BC,
 H5BD), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B)
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), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
6.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C)
Attempts at such refinement on the disordered MeCN (C32A, C32B) did not 
converge and these hydrogens were therefore not modelled.
;
_shelx_res_checksum              46437
_olex2_submission_special_instructions 'No special instructions were received'