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_7247455
_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         'C25 H24 Mn N4 O5'
_chemical_formula_sum            'C25 H24 Mn N4 O5'
_chemical_formula_weight         515.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-08
_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                 93.831(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8278(3)
_cell_length_b                   14.7244(3)
_cell_length_c                   7.7390(2)
_cell_measurement_reflns_used    11405
_cell_measurement_temperature    299.6(7)
_cell_measurement_theta_max      28.9540
_cell_measurement_theta_min      3.9000
_cell_volume                     2368.07(9)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.6(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.947
_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    -25.00  61.00   1.00   25.00    --   18.87 -99.00  30.00   86
  2  \w    -50.00  40.00   1.00   25.00    --   18.87 -57.00  90.00   90
  3  \w    -25.00  61.00   1.00   25.00    --   18.87 -99.00 -90.00   86
  4  \w    -25.00  61.00   1.00   25.00    --   18.87 -99.00-180.00   86
  5  \w    -88.00   2.00   1.00   25.00    --  -19.50 -57.00-150.00   90
  6  \w    -88.00   2.00   1.00   25.00    --  -19.50 -57.00   0.00   90
  7  \w    -41.00  49.00   1.00   25.00    --  -19.50  57.00   0.00   90
  8  \w    -90.00  11.00   1.00   25.00    --  -19.50 -77.00 -30.00  101
  9  \w    -90.00  11.00   1.00   25.00    --  -19.50 -77.00 120.00  101
 10  \w    -25.00  61.00   1.00   25.00    --   18.87 -99.00 -30.00   86
 11  \w    -50.00  40.00   1.00   25.00    --   18.87 -57.00-120.00   90
 12  \w    -25.00  61.00   1.00   25.00    --   18.87 -99.00  60.00   86
 13  \w    -50.00  51.00   1.00   25.00    --  -19.50  77.00 150.00  101
 14  \w    -41.00  49.00   1.00   25.00    --  -19.50  57.00-180.00   90
 15  \w    -90.00  11.00   1.00   25.00    --  -19.50 -77.00 150.00  101
 16  \w    -25.00  22.00   1.00   25.00    --  -19.50 -99.00-150.00   47
 17  \w    -54.00  92.00   1.00   25.00    --   18.87   0.00-150.00  146
 18  \w    -54.00  92.00   1.00   25.00    --   18.87   0.00-180.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0314335000
_diffrn_orient_matrix_UB_12      0.0148904000
_diffrn_orient_matrix_UB_13      -0.0160298000
_diffrn_orient_matrix_UB_21      0.0039288000
_diffrn_orient_matrix_UB_22      -0.0383568000
_diffrn_orient_matrix_UB_23      -0.0537435000
_diffrn_orient_matrix_UB_31      -0.0126989000
_diffrn_orient_matrix_UB_32      0.0250433000
_diffrn_orient_matrix_UB_33      -0.0727684000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            41137
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.413
_diffrn_reflns_theta_min         3.391
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98094
_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    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.143
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         3106
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0420P)^2^+1.2323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2434
_reflns_number_total             3106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00881a2.cif
_cod_data_source_block           mnmofsandbath72h
_cod_depositor_comments
'Adding full bibliography for 7247455--7247462.cif.'
_cod_database_code               7247455
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H75N4O4Mn3
_chemical_oxdiff_usercomment     'cubic crystal'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Mn1-H30A \\sim Mn1-H30B
 with sigma of 0.02
3. Others
 Fixed Sof: H30A(0.5) H30B(0.5) H1A(0.5) H1B(0.5)
4.a Free rotating group:
 O30(H30A,H30B)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C23(H23), C26(H26), C22(H22)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              14209
_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 1.024
_oxdiff_exptl_absorpt_empirical_full_min 0.965