Understanding the structural landscape of Mn-based MOFs formed with hinged pyrazole carboxylate linkers
Smernik, Josephine F.; Gimeno-Fonquernie, Pol; Albalad, Jorge; Jones, Tyla S.; Young, Rosemary J.; Champness, Neil R.; Doonan, Christian J.; Evans, Jack D.; Sumby, Christopher J.; CrystEngComm 25 (2023) 6539–6548; doi:10.1039/D3CE00881A

data_7247462
_publ_section_title
;
 Understanding the structural landscape of Mn-based MOFs formed with
 hinged pyrazole carboxylate linkers
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              6539
_journal_page_last               6548
_journal_paper_doi               10.1039/D3CE00881A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C26 H36 Mn2 N8 O12'
_chemical_formula_sum            'C26 H36 Mn2 N8 O12'
_chemical_formula_weight         762.51
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-23 deposited with the CCDC.	2023-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.13640(10)
_cell_length_b                   16.5273(3)
_cell_length_c                   21.5295(3)
_cell_measurement_reflns_used    8346
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8210
_cell_measurement_theta_min      3.8140
_cell_volume                     3182.28(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1695
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.879
_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    -54.00  63.00   0.75   40.00    --   18.87 -19.00  30.00  156
  2  \w    -25.00  21.50   0.75   40.00    --  -19.50 -99.00 -60.00   62
  3  \w    -95.00 -35.00   0.75   40.00    --  -19.50-178.00-180.00   80
  4  \w    -50.00  50.50   0.75   40.00    --  -19.50  77.00  90.00  134
  5  \w    -41.00 -15.50   0.75   40.00    --  -19.50  57.00-150.00   34
  6  \w    -90.00  10.50   0.75   40.00    --  -19.50 -77.00  90.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28904
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.403
_diffrn_reflns_theta_min         3.357
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7736
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+3.0717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6122
_reflns_number_total             7736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00881a2.cif
_cod_data_source_block           jsx02
_cod_depositor_comments
'Adding full bibliography for 7247455--7247462.cif.'
_cod_database_code               7247462
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.763
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H,H) groups, All Mn(H,H,H,H)
  groups
2. Restrained distances
 O64-H64B
 -0.95 with sigma of 0.02
 O61-H61B
 -0.95 with sigma of 0.02
 O62-H62B
 -0.95 with sigma of 0.02
 O63-H63B
 -0.95 with sigma of 0.02
 O64-H64A
 -0.95 with sigma of 0.02
 O61-H61A
 -0.95 with sigma of 0.02
 O62-H62A
 -0.95 with sigma of 0.02
 O63-H63A
 -0.95 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C31(H31A,H31B)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C)
;
_shelx_res_checksum              26423
_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
;