In-Depth Magnetic Characterization of a [2 × 2] Mn(III) Square Grid Using SQUID Magnetometry, Inelastic Neutron Scattering, and High-Field Electron Paramagnetic Resonance Spectroscopy.
Konstantatos, Andreas; Bewley, Robert; Barra, Anne-Laure; Bendix, Jesper; Piligkos, Stergios; Weihe, Høgni; Inorganic chemistry 55 (2016) 10377–10382; doi:10.1021/acs.inorgchem.6b01634

data_4348791
_publ_section_title
;
 In-Depth Magnetic Characterization of a [2 \\times 2] Mn(III) Square Grid
 Using SQUID Magnetometry, Inelastic Neutron Scattering, and High-Field
 Electron Paramagnetic Resonance Spectroscopy.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10377
_journal_page_last               10382
_journal_paper_doi               10.1021/acs.inorgchem.6b01634
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C32 H30 Mn2 N4 O8, C3 H7 N O'
_chemical_formula_sum            'C35 H37 Mn2 N5 O9'
_chemical_formula_weight         781.59
_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_Int_Tables_number      15
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.793(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.7556(14)
_cell_length_b                   12.9539(8)
_cell_length_c                   22.6368(12)
_cell_measurement_reflns_used    7893
_cell_measurement_temperature    123
_cell_measurement_theta_max      24.81
_cell_measurement_theta_min      2.18
_cell_volume                     6594.6(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.0
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44496
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1084 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.9414.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.5743
_exptl_crystal_description       block
_exptl_crystal_F_000             3239.0335
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.6356
_refine_diff_density_min         -0.4753
_refine_diff_density_rms         0.1177
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             9.4192
_refine_ls_goodness_of_fit_ref   1.0692
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    62
_refine_ls_number_parameters     465
_refine_ls_number_reflns         5825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0692
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+6.8371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              26
_reflns_limit_h_min              -28
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                4527
_reflns_number_total             5825
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic6b01634_si_002.cif
_cod_data_source_block           mo_D8V575_0m-1
_cod_database_code               4348791
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C39(H39), C40(H40), C43(H43),
  C44(H44), C45(H45), C48(H48), C49(H49)
2.b Idealised Me refined as rotating group:
 C38(H38a,H38b,H38c), C41(H41a,H41b,H41c), C42(H42a,H42b,H42c), C47(H47a,H47b,
 H47c), C50(H50a,H50b,H50c), C51(H51a,H51b,H51c)
;
_olex2_submission_original_sample_id AKH144
_olex2_submission_special_instructions 'No special instructions were received'