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_7247461
_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         'C21 H13 Mn N4 O4, 0.833(C3 H7 N O)'
_chemical_formula_sum            'C23.5 H18.83 Mn N4.83 O4.83'
_chemical_formula_weight         501.22
_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   geom
_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                 114.461(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.2881(7)
_cell_length_b                   10.4868(2)
_cell_length_c                   24.8587(8)
_cell_measurement_reflns_used    11149
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3910
_cell_measurement_theta_min      3.9000
_cell_volume                     5526.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_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_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_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   -121.00 -39.00   0.50    4.76    --  -48.52 -35.00-173.00  164
  2  \w    -37.00  24.00   0.50    4.76    --  -48.52  35.00 -16.00  122
  3  \w     39.00 121.00   0.50    4.76    --   48.52  35.00 -16.00  164
  4  \w    -24.00  35.00   0.50    4.76    --   48.52 -35.00-173.00  118
  5  \w   -163.00 -79.00   0.50   19.03    --  -90.00 -35.00-173.00  168
  6  \w     96.00 178.00   0.50   19.03    --  106.92  35.00 -16.00  164
  7  \w    -17.00  26.00   0.50    4.76    --  -48.52  19.00 120.00   86
  8  \w   -120.00 -94.00   0.50    4.76    --  -48.52-125.00   0.00   52
  9  \w    -17.00  26.00   0.50    4.76    --  -48.52  19.00-120.00   86
 10  \w    -24.00  39.00   0.50    4.76    --   48.52 -38.00  60.00  126
 11  \w   -161.00-110.00   0.50   19.03    --  -90.00 -77.00 120.00  102
 12  \w    -85.00 -18.00   0.50   19.03    --  -90.00 125.00  60.00  134
 13  \w    -68.00 -18.00   0.50   19.03    --  -90.00  57.00  90.00  100
 14  \w   -161.00-106.00   0.50   19.03    --  -90.00 -99.00 -30.00  110
 15  \w     35.00 111.00   0.50   19.03    --  106.92-125.00  90.00  152
 16  \w     35.00 106.00   0.50   19.03    --  106.92 -99.00   0.00  142
 17  \w     35.00  66.00   0.50   19.03    --  106.92 -57.00  90.00   62
 18  \w     95.00 178.00   0.50   19.03    --  106.92 125.00-180.00  166
 19  \w     35.00  66.00   0.50   19.03    --  106.92 -57.00-150.00   62
 20  \w     35.00  66.00   0.50   19.03    --  106.92 -57.00 -30.00   62
 21  \w    118.00 173.00   0.50   19.03    --  106.92  57.00  60.00  110
 22  \w     36.00  62.00   0.50   19.03    --  106.92 -57.00-120.00   52
 23  \w     35.00  66.00   0.50   19.03    --  106.92 -57.00 150.00   62
 24  \w    110.00 178.00   0.50   19.03    --  106.92  38.00  30.00  136
 25  \w     35.00  60.00   0.50   19.03    --  106.92 -57.00 -60.00   50
 26  \w     38.00  65.00   0.50   19.03    --  106.92 -57.00 -90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0154517000
_diffrn_orient_matrix_UB_12      -0.0042304000
_diffrn_orient_matrix_UB_13      -0.0665576000
_diffrn_orient_matrix_UB_21      0.0636551000
_diffrn_orient_matrix_UB_22      -0.0660704000
_diffrn_orient_matrix_UB_23      0.0137822000
_diffrn_orient_matrix_UB_31      -0.0315118000
_diffrn_orient_matrix_UB_32      -0.1310544000
_diffrn_orient_matrix_UB_33      -0.0047283000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26454
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.511
_diffrn_reflns_theta_min         3.907
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.54a (Rigaku Oxford Diffraction, 2022)
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    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             2059
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5632
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1788P)^2^+9.1894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2457
_refine_ls_wR_factor_ref         0.2577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4617
_reflns_number_total             5632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00881a2.cif
_cod_data_source_block           mn_pl8_auto
_cod_depositor_comments
'Adding full bibliography for 7247455--7247462.cif.'
_cod_original_formula_sum        'C23.50 H18.83 Mn N4.83 O4.83'
_cod_database_code               7247461
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     DMF
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
N40 \\sim C41 \\sim C42 \\sim C43 \\sim O44: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O30 \\sim N31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 N40, C41, C42, C43, O44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O30, N31, C32, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N40(0.33333) O30(0.5) N31(0.5) C32(0.5) H32(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
 C41(0.33333) H41A(0.33333) H41B(0.33333) H41C(0.33333) C42(0.33333)
 H42(0.33333) C43(0.33333) H43A(0.33333) H43B(0.33333) H43C(0.33333)
 O44(0.33333)
5.a Ternary CH refined with riding coordinates:
 C24(H24)
5.b Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C)
5.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C25(H25), C7(H7), C15(H15), C19(H19), C26(H26), C30(H30), C29(H29),
 C16(H16), C27(H27), C4(H4), C2(H2), C32(H32), C42(H42)
5.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              49062
_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 1.730
_oxdiff_exptl_absorpt_empirical_full_min 0.747