Computational Studies of the Magneto-structural Correlations in a Manganese Dimer with Jahn-Teller Distortions
Buchanan, Jenna; Dais, Tyson N.; Plieger, Paul; Physical Chemistry Chemical Physics  (2022) –; doi:10.1039/D1CP05514C

data_7244315
_publ_section_title
;
 Computational Studies of the Magneto-structural Correlations in a
 Manganese Dimer with Jahn-Teller Distortions
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D1CP05514C
_journal_year                    2022
_chemical_formula_moiety
'C68 H91.2 Mn2 N5.2 O10, 3(Cl O4), 1[ClO4-], 3[C2H3N], 4[H2O]'
_chemical_formula_sum            'C74 H108.2 Cl4 Mn2 N8.2 O30'
_chemical_formula_weight         1844.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-10-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2021-11-29 deposited with the CCDC.	2022-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                92.892(7)
_cell_angle_beta                 93.983(7)
_cell_angle_gamma                98.707(7)
_cell_formula_units_Z            2
_cell_length_a                   9.5605(2)
_cell_length_b                   15.8753(3)
_cell_length_c                   31.531(2)
_cell_measurement_reflns_used    47515
_cell_measurement_temperature    153
_cell_measurement_theta_max      72.1
_cell_measurement_theta_min      6.6
_cell_volume                     4710.0(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153
_diffrn_detector                 'Curved Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_unetI/netI     0.1340
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            81849
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        65.074
_diffrn_reflns_theta_max         65.074
_diffrn_reflns_theta_min         6.563
_diffrn_source                   'rotating anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Cu
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.882
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   EMPIRICAL
_exptl_crystal_colour            Black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1935
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         15384
_refine_ls_number_restraints     382
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.1206
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3141
_refine_ls_wR_factor_ref         0.3860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6823
_reflns_number_total             15384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp05514c2.cif
_cod_data_source_block           jkb
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Black' was changed
to 'black' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        4710.0(4)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C74 H108.20 Cl4 Mn2 N8.20 O30'
_cod_database_code               7244315
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.274
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H00C of O00C, H00A of O00A, All C(H,H) groups, All N(H)
  groups
 At 1.5 times of:
  All C(H,H,H) groups, H02Z of O02H, H02 of O02M
2. Restrained distances
 C01L-O1
 1.23 with sigma of 0.02
 C02C-O00K
 1.23 with sigma of 0.02
 C2-C4 \\sim C2-C6
 with sigma of 0.04
 C3-C17 \\sim C3-C18 \\sim C3-C19
 with sigma of 0.04
 C7-C9 \\sim C7-C11
 with sigma of 0.04
 C13-C14 \\sim C13-C15 \\sim C13-C16 \\sim C13-C12
 with sigma of 0.02
 C14-C15 \\sim C14-C16 \\sim C15-C16
 with sigma of 0.04
 C12-C14 \\sim C12-C15 \\sim C12-C16
 with sigma of 0.04
 C5-C17 \\sim C5-C18 \\sim C5-C19 \\sim C5-C3
 with sigma of 0.02
 C17-C18 \\sim C17-C19 \\sim C18-C19
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C2 \\sim C4 \\sim C6: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C7 \\sim C9 \\sim C11: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C3 \\sim C5 \\sim C17 \\sim C18 \\sim C19: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(Cl04) \\sim Ueq, Uanis(O02A) \\sim Ueq, Uanis(O02N) \\sim Ueq,
Uanis(O02S) \\sim Ueq, Uanis(O02V) \\sim Ueq, Uanis(Cl03) \\sim Ueq,
Uanis(O011) \\sim Ueq, Uanis(O02G) \\sim Ueq, Uanis(O02T) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(Cl05) \\sim Ueq, Uanis(O00I) \\sim Ueq, Uanis(O013) \\sim Ueq,
Uanis(O019) \\sim Ueq, Uanis(O01E) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C4) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C02Q) \\sim Ueq, Uanis(C02P) \\sim Ueq, Uanis(C02D)
\\sim Ueq, Uanis(C01L) \\sim Ueq, Uanis(C023) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C02B) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N00J) \\sim Ueq, Uanis(N00F) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O00K) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C2, C4, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C9, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C5, C17, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N00F(0.6) N00J(0.6) H01L(0.6) H01I(0.4) H02W(0.4) H02V(0.6)
 O02H(0.6) H02Z(0.6) O02M(0.6) H02(0.6) O1(0.4) O00K(0.4) C2(0.66667)
 H2A(0.66667) H2B(0.66667) H2C(0.66667) C4(0.66667) H4A(0.66667) H4B(0.66667)
 H4C(0.66667) C6(0.66667) H6A(0.66667) H6B(0.66667) H6C(0.66667) C7(0.66667)
 H7A(0.66667) H7B(0.66667) H7C(0.66667) C9(0.66667) H9A(0.66667) H9B(0.66667)
 H9C(0.66667) C11(0.66667) H11A(0.66667) H11B(0.66667) H11C(0.66667)
 C12(0.33333) H12A(0.33333) H12B(0.33333) H12C(0.33333) C14(0.33333)
 H14A(0.33333) H14B(0.33333) H14C(0.33333) C15(0.33333) H15A(0.33333)
 H15B(0.33333) H15C(0.33333) C3(0.33333) H3A(0.33333) H3B(0.33333) H3C(0.33333)
 C18(0.33333) H18A(0.33333) H18B(0.33333) H18C(0.33333) C19(0.33333)
 H19A(0.33333) H19B(0.33333) H19C(0.33333)
 Fixed U11: O1(0.104352) O00K(0.059302)
 Fixed U12: O1(-0.006488) O00K(0.01722)
 Fixed U13: O1(0.018743) O00K(0.002597)
 Fixed U22: O1(0.117342) O00K(0.055341)
 Fixed U23: O1(-0.015014) O00K(0.008883)
 Fixed U33: O1(0.10456) O00K(0.05878)
 Fixed X: O1(0.57102) O00K(0.291301)
 Fixed Y: O1(0.442729) O00K(0.51501)
 Fixed Z: O1(0.663161) O00K(0.64721)
6.a Free rotating group:
 C2(C4,C6), C7(C9,C11)
6.b Ternary CH refined with riding coordinates:
 N00E(H00E), N00G(H00G), N00H(H00H), N00O(H00O)
6.c Secondary CH2 refined with riding coordinates:
 C00U(H00B,H00D), C015(H01B,H01C), C01P(H01P,H01Q), C01S(H01S,H01T), C01T(H01U,
 H01V), C01V(H01W,H01X), C01X(H01Z,HB), C02D(H02X,H02Y)
6.d Aromatic/amide H refined with riding coordinates:
 O00A(H00A), O00C(H00C), C00Q(H00Q), C00K(H00K), C01A(H01A), C017(H017),
 C00Z(H00Z), C010(H010), C00V(H00V), C01O(H01O), C018(H018), C00X(H00X),
 C01D(H01D), C01H(H01H), C01J(H01J), C01R(H01R), C02B(H02B), C023(H023),
 C01L(H01L), C01L(H01I), C02P(H02P), C02Q(H02Q), C02C(H02W), C02C(H02V)
6.e Fitted hexagon refined as free rotating group:
 C00P(C00M,C00R,C00Q,C00Y,C00K), C00S(C01A,C017,C01I,C00Z,C010), C00W(C00N,
 C01O,C012,C018,C00T), C016(C01D,C01H,C01G,C01J,C01R), C01C(C01U,C02B,C17,C023,
 C01Q), C024(C01K,C026,C02P,C16,C02Q)
6.f Idealised Me refined as rotating group:
 C01F(H01E,H01F,H01G), C01N(H01K,H01M,H01N), C01W(H01Y,H,HA), C01Z(H01,HC,HD),
 C020(H02A,H02C,H02D), C021(H02E,H02F,H02G), C022(H02H,H02I,H02J), C025(H02K,
 H02L,H02M), C027(H02N,H02O,H02R), C028(H02S,H02T,H02U), C2(H2A,H2B,H2C),
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C3(H3A,H3B,H3C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
6.g Idealised tetrahedral OH refined as rotating group:
 O02H(H02Z), O02M(H02)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 302 electrons were 
found in a volume of 1438\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[ClO4-], 3[C2H3N], 4[H2O] per Asymmetric Unit 
which account for 310 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49852
_shelx_hkl_checksum              50645
_shelx_fab_checksum              85494
_olex2_submission_special_instructions 'No special instructions were received'