A hexagon based Mn(II) rod metal-organic framework - structure, SF<sub>6</sub> gas sorption, magnetism and electrochemistry.
Amombo Noa, Francoise M.; Cheung, Ocean; Åhlén, Michelle; Ahlberg, Elisabet; Nehla, Priyanka; Salazar-Alvarez, Germán; Ershadrad, Soheil; Sanyal, Biplab; Öhrström, Lars; Chemical communications (Cambridge, England) 59 (2023) 2106–2109; doi:10.1039/d2cc06916d

data_7131215
_publ_section_title
;
 A hexagon based Mn(II) rod metal-organic framework - structure,
 SF<sub>6</sub> gas sorption, magnetism and electrochemistry.
;
_journal_issue                   15
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2106
_journal_page_last               2109
_journal_paper_doi               10.1039/d2cc06916d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C57 H45 Mn3 N3 O15'
_chemical_formula_sum            'C57 H45 Mn3 N3 O15'
_chemical_formula_weight         1176.78
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-14
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2023-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.990(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5886(2)
_cell_length_b                   27.8179(4)
_cell_length_c                   16.6789(3)
_cell_measurement_reflns_used    23919
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.1400
_cell_measurement_theta_min      3.1120
_cell_volume                     5259.48(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -119.00 -30.00   0.50    9.28    --  -43.20 -46.00  47.00  178
  2  \w    -32.00  34.00   0.50    9.28    --   43.20 -46.00  47.00  132
  3  \w     30.00 119.00   0.50    9.28    --   43.20  46.00-163.00  178
  4  \w   -174.00 -91.00   0.50   37.13    -- -104.50 -46.00  47.00  166
  5  \w     96.00 178.00   0.50   37.13    --  109.23  46.00-163.00  164
  6  \w    -27.00  32.00   0.50    9.28    --  -43.20  46.00-163.00  118
  7  \w    -15.00  34.00   0.50    9.28    --  -43.20  38.00 -30.00   98
  8  \w      3.00  77.00   0.50    9.28    --   43.20 -99.00-180.00  148
  9  \w    -34.00  22.00   0.50    9.28    --   43.20 -38.00 -60.00  112
 10  \w      3.00  77.00   0.50    9.28    --   43.20 -99.00  90.00  148
 11  \w    -72.00 -30.00   0.50   37.13    -- -104.50  77.00  60.00   84
 12  \w    -72.00 -30.00   0.50   37.13    -- -104.50  77.00 -90.00   84
 13  \w    -72.00 -30.00   0.50   37.13    -- -104.50  77.00 -60.00   84
 14  \w   -132.00 -89.00   0.50   37.13    -- -104.50 -15.00  90.00   86
 15  \w    -72.00 -30.00   0.50   37.13    -- -104.50  77.00-180.00   84
 16  \w   -174.00-103.00   0.50   37.13    -- -104.50 -77.00 150.00  142
 17  \w   -174.00-103.00   0.50   37.13    -- -104.50 -95.00-180.00  142
 18  \w    -72.00 -30.00   0.50   37.13    -- -104.50  77.00 150.00   84
 19  \w    -72.00 -30.00   0.50   37.13    -- -104.50  77.00  30.00   84
 20  \w     35.00  93.00   0.50   37.13    --  109.23 -95.00 120.00  116
 21  \w     36.00 101.00   0.50   37.13    --  109.23-125.00 -90.00  130
 22  \w     94.00 139.00   0.50   37.13    --  109.23  15.00 -60.00   90
 23  \w     35.00  79.00   0.50   37.13    --  109.23 -77.00-150.00   88
 24  \w     35.00  79.00   0.50   37.13    --  109.23 -77.00  60.00   88
 25  \w     35.00  79.00   0.50   37.13    --  109.23 -77.00 -90.00   88
 26  \w     35.00  79.00   0.50   37.13    --  109.23 -77.00   0.00   88
 27  \w     94.00 139.00   0.50   37.13    --  109.23  15.00   0.00   90
 28  \w     30.00 120.00   0.50    9.28    --   43.20  38.00 -30.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0093501000
_diffrn_orient_matrix_UB_12      0.0169034000
_diffrn_orient_matrix_UB_13      0.0863692000
_diffrn_orient_matrix_UB_21      0.1151614000
_diffrn_orient_matrix_UB_22      -0.0268392000
_diffrn_orient_matrix_UB_23      0.0367063000
_diffrn_orient_matrix_UB_31      0.0715566000
_diffrn_orient_matrix_UB_32      0.0453971000
_diffrn_orient_matrix_UB_33      -0.0104909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48937
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.657
_diffrn_reflns_theta_min         3.140
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.391
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.104
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.538
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.742
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10616
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.1176
_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^)+(0.1285P)^2^+93.4207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3164
_refine_ls_wR_factor_ref         0.3216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9060
_reflns_number_total             10616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06916d2.cif
_cod_data_source_block           CTH-18
_cod_depositor_comments          'Adding full bibliography for 7131215.cif.'
_cod_database_code               7131215
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C228  H180  Mn12  N12  O60  '
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.130
_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. Restrained distances
 N12-C60
 1.5 with sigma of 0.002
 N17-C66
 1.5 with sigma of 0.002
 C53-N65
 1.331 with sigma of 0.002
 N65-C59
 1.459 with sigma of 0.002
 N65-C61
 1.45 with sigma of 0.002
 O17-C61
 2.795 with sigma of 0.002
 C61-C59
 2.486 with sigma of 0.002
 C53-C59
 2.434 with sigma of 0.002
 C62-N18
 1.331 with sigma of 0.002
 N18-C63
 1.459 with sigma of 0.002
 N18-C64
 1.45 with sigma of 0.002
 O16-C64
 2.795 with sigma of 0.002
 C63-C64
 2.486 with sigma of 0.002
 C62-C63
 2.434 with sigma of 0.002
3. Others
 Sof(C54)=Sof(H54A)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H54B)=Sof(C60)=Sof(H60A)=
 Sof(H60B)=Sof(H60C)=Sof(N12)=1-FVAR(1)
 Sof(N2)=Sof(C52)=Sof(H52A)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56)=
 Sof(H52B)=Sof(H56A)=Sof(H56B)=FVAR(1)
 Sof(C57)=Sof(H57)=Sof(O15)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C66)=
 Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(N17)=1-FVAR(2)
 Sof(O13)=Sof(N1)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=FVAR(2)
 Sof(C53)=Sof(H53)=Sof(O17)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C61)=
 Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(N65)=1-FVAR(3)
 Sof(O16)=Sof(N18)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(3)
4.a Aromatic/amide H refined with riding coordinates:
 C43(H43), C26(H26), C15(H15), C8(H8), C47(H47), C44(H44), C33(H33), C36(H36),
 C40(H40), C30(H30), C46(H46), C29(H29), C19(H19), C11(H11), C39(H39), C32(H32),
  C16(H16), C12(H12), C37(H37), C9(H9), C18(H18), C25(H25), C22(H22), C23(H23),
 C49(H49), C52(H52A), C54(H54A), C57(H57), C53(H53), C62(H62)
4.b Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C55(H55A,H55B,H55C), C56(H52B,H56A,
 H56B), C58(H58A,H58B,H54B), C60(H60A,H60B,H60C), C65(H65A,H65B,H65C), C66(H66A,
 H66B,H66C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C)
;
_shelx_res_checksum              85163
_shelx_hkl_checksum              30826
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.472
_oxdiff_exptl_absorpt_empirical_full_min 0.640