Slow magnetic relaxation in a dimeric Mn2Ca2 complex enabled by the large Mn(iii) rhombicity.
Arauzo, Ana; Bartolomé, Elena; Benniston, Andrew C.; Melnic, Silvia; Shova, Sergiu; Luzón, Javier; Alonso, Pablo J.; Barra, Anne-Laure; Bartolomé, Juan; Dalton transactions (Cambridge, England : 2003) 46 (2017) 720–732; doi:10.1039/c6dt02509a

data_7041365
_publ_section_title
;
 Slow magnetic relaxation in a dimeric Mn2Ca2 complex enabled by the large
 Mn(iii) rhombicity.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              720
_journal_page_last               732
_journal_paper_doi               10.1039/c6dt02509a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C40 H50 Ca2 Mn2 N8 O10, 4(Cl O4), 2(C2 H3 N)'
_chemical_formula_sum            'C44 H56 Ca2 Cl4 Mn2 N10 O26'
_chemical_formula_weight         1472.83
_chemical_name_systematic
;
 ? 
;
_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             2015-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-06-01 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.253(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.6073(11)
_cell_length_b                   14.4511(5)
_cell_length_c                   16.2615(7)
_cell_measurement_reflns_used    3439
_cell_measurement_temperature    260.00(14)
_cell_measurement_theta_max      24.9160
_cell_measurement_theta_min      1.6030
_cell_volume                     6435.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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, 2008)'
_diffrn_ambient_temperature      260.00(14)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -22.00   15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1690  -99.0000   60.0000 37

  2 omega   -3.00   78.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690   19.0000  150.0000 81

  3 omega  -51.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690  -19.0000  -60.0000 108
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0231672000
_diffrn_orient_matrix_UB_12      -0.0160789000
_diffrn_orient_matrix_UB_13      0.0082965000
_diffrn_orient_matrix_UB_21      -0.0079675000
_diffrn_orient_matrix_UB_22      -0.0019354000
_diffrn_orient_matrix_UB_23      -0.0431847000
_diffrn_orient_matrix_UB_31      0.0083403000
_diffrn_orient_matrix_UB_32      -0.0463528000
_diffrn_orient_matrix_UB_33      -0.0010270000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12656
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.59
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.092
_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     394
_refine_ls_number_reflns         5681
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+19.9101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                3994
_reflns_number_total             5681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02509a2.cif
_cod_data_source_block           shi_2586_sime
_cod_depositor_comments          'Adding full bibliography for 7041365.cif.'
_cod_database_code               7041365
_chemical_oxdiff_formula         'C20 H20 N6 O18 Cl1 Mn2 Ca1'
_chemical_oxdiff_usercomment     'OEC_19 rep._2435'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Cl3-O8 \\sim Cl3-O9 \\sim Cl3-O11X \\sim Cl3-O11 \\sim Cl3-O10
 with sigma of 0.01
 Cl3-O8 \\sim Cl3-O11X \\sim Cl3-O11 \\sim Cl3-O10 \\sim Cl3-O9 \\sim Cl2-O5X
\\sim Cl2-O5 \\sim Cl2-O6 ~
 Cl2-O4X \\sim Cl2-O4 \\sim Cl2-O7 \\sim Cl2-O7X \\sim Cl2-O6X \\sim Cl1-O13X
\\sim Cl1-O14 \\sim Cl1-O13 ~
 Cl1-O12 \\sim Cl1-O12X \\sim Cl1-O15
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(O12) = Uiso(O13) = Uiso(O15) = Uiso(O14) = Uiso(O12X) = Uiso(O13X)
Uiso(O10) = Uiso(O11) = Uiso(O11X) = Uiso(O8) = Uiso(O9)
Uiso(O5X) = Uiso(O4X) = Uiso(O4) = Uiso(O5) = Uiso(O7) = Uiso(O7X) = Uiso(O6X)
4. Others
 Fixed Sof: O5(0.5) O5X(0.35) O6X(0.25) O7(0.5) O7X(0.5) O4(0.5) O4X(0.4)
 O13X(0.25) O15(0.3) O12X(0.3) O14(0.3) O12(0.6) O13(0.25) O10(0.4) O8(0.4)
 O11(0.4) O9(0.4) O11X(0.4)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C)
;
_olex2_date_sample_data_collection 2014-06-06
_olex2_submission_special_instructions 'No special instructions were received'