Switching the orientation of Jahn-Teller axes in oxime-based Mn(III) dimers and its effect upon magnetic exchange: a combined experimental and theoretical study.
Comar, Priyanka; Rajeshkumar, Thayalan; Nichol, Gary S.; Pitak, Mateusz B.; Coles, Simon J.; Rajaraman, Gopalan; Brechin, Euan K.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19805–19811; doi:10.1039/c5dt03615a

data_7036850
_publ_section_title
;
 Switching the orientation of Jahn-Teller axes in oxime-based Mn(III)
 dimers and its effect upon magnetic exchange: a combined experimental and
 theoretical study.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19805
_journal_page_last               19811
_journal_paper_doi               10.1039/c5dt03615a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C38 H36 Mn2 N8 O4, 2(Cl1 O4)'
_chemical_formula_sum            'C40 H44 Cl2 Mn2 N8 O14'
_chemical_formula_weight         1041.61
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_audit_update_record
;
2015-01-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.936(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2526(7)
_cell_length_b                   22.2504(12)
_cell_length_c                   15.7127(11)
_cell_measurement_reflns_used    4853
_cell_measurement_temperature    120
_cell_measurement_theta_max      51.9940
_cell_measurement_theta_min      3.4640
_cell_volume                     4442.3(5)
_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, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.600
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0315335000
_diffrn_orient_matrix_UB_12      0.0667725000
_diffrn_orient_matrix_UB_13      -0.0175412000
_diffrn_orient_matrix_UB_21      -0.1081829000
_diffrn_orient_matrix_UB_22      -0.0152547000
_diffrn_orient_matrix_UB_23      -0.0058748000
_diffrn_orient_matrix_UB_31      0.0447155000
_diffrn_orient_matrix_UB_32      0.0100507000
_diffrn_orient_matrix_UB_33      0.1084215000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_laue_measured_fraction_full 0.600
_diffrn_reflns_laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19662
_diffrn_reflns_point_group_measured_fraction_full 0.600
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         52.004
_diffrn_reflns_theta_min         3.478
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.388
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.0705
_exptl_crystal_size_min          0.0264
_platon_squeeze_details          '2 MeOH per asymmetric unit removed'
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1144P)^2^+3.1849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.2073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3243
_reflns_number_total             4819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03615a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7036847--7036851.cif.'
_cod_database_code               7036850
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H40 N4 O20 Mn3 Cl4'
_chemical_oxdiff_usercomment     '@ 120 K PC152b'
_reflns_odcompleteness_completeness 98.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_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 N(H) groups
2. Rigid bond restraints
 Cl2', O9', O10', O11', O12'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Cl2' \\sim O9' \\sim O10' \\sim O11' \\sim O12': within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl2', O10'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{Cl2, O9, O10, O11, O12}
as
{Cl2', O9', O10', O11', O12'}
6. Others
 Sof(Cl2')=Sof(O9')=Sof(O10')=Sof(O11')=Sof(O12')=1-FVAR(1)
 Sof(Cl2)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 N5(H5), N8(H8)
7.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C26(H26A,H26B), C32(H32A,H32B), C38(H38A,H38B)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5A), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
  C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22),
 C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
  C35(H35), C36(H36)
;
_shelx_res_checksum              57695
_shelx_fab_checksum              37696