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_7036851
_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         'C50 H44 Mn2 N8 O4, 2(Cl O4), 1.61(C4 H8 O1)'
_chemical_formula_sum            'C56.44 H56.87 Cl2 Mn2 N8 O13.61'
_chemical_formula_weight         1245.74
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-11-29
_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                110.595(3)
_cell_angle_beta                 103.803(4)
_cell_angle_gamma                92.048(3)
_cell_formula_units_Z            1
_cell_length_a                   8.4822(4)
_cell_length_b                   13.2500(4)
_cell_length_c                   13.6070(5)
_cell_measurement_reflns_used    9349
_cell_measurement_temperature    120
_cell_measurement_theta_max      75.8080
_cell_measurement_theta_min      4.0180
_cell_volume                     1378.11(10)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0298347000
_diffrn_orient_matrix_UB_12      0.0211278000
_diffrn_orient_matrix_UB_13      0.1221857000
_diffrn_orient_matrix_UB_21      0.0305556000
_diffrn_orient_matrix_UB_22      -0.1189352000
_diffrn_orient_matrix_UB_23      -0.0222326000
_diffrn_orient_matrix_UB_31      0.1837671000
_diffrn_orient_matrix_UB_32      0.0332770000
_diffrn_orient_matrix_UB_33      0.0184659000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21371
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.336
_diffrn_reflns_theta_min         3.595
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.247
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.971
_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    1.501
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.3496
_exptl_crystal_size_mid          0.0523
_exptl_crystal_size_min          0.0464
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5662
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0817P)^2^+1.4581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5040
_reflns_number_total             5662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03615a2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7036847--7036851.cif.'
_cod_original_cell_volume        1378.12(10)
_cod_database_code               7036851
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C30 H40 N8 O20 Mn2 Cl'
_chemical_oxdiff_usercomment     '@ 120 K PC490'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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) groups
2. Restrained distances
 C28-C27
 1.47 with sigma of 0.02
 C29-C28 = C27-C26
 1.48 with sigma of 0.02
 O7-C29 = O7-C26
 1.44 with sigma of 0.02
 N4-H4
 0.84 with sigma of 0.01
3. Rigid bond restraints
 O7, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O7, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C14, C15, C16, C17, C18, C19, N4, C25, C24, C23, C22, C21, C20, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C29 \\sim O7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O7 \\sim C26: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N2 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim N4 \\sim
C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim N3: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(O7)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,
 H28B), C29(H29A,H29B)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
 C23(H23), C3(H3), C2(H2), C9(H9), C13(H13), C4(H4A), C5(H5), C10(H10),
 C12(H12), C11(H11)
;
_shelx_res_checksum              18845