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_7247460
_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 H23 Mn2 N9 O11'
_chemical_formula_sum            'C21 H23 Mn2 N9 O11'
_chemical_formula_weight         687.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 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                 107.377(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.318(3)
_cell_length_b                   12.9645(13)
_cell_length_c                   9.0482(12)
_cell_measurement_reflns_used    16561
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1620
_cell_measurement_theta_min      3.8850
_cell_volume                     1379.0(4)
_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_temperature      293(2)
_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 0.931
_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    -11.00  89.00   1.00   10.00    --   19.03  77.00  30.00  100
  2  \w    -53.00  45.00   1.00   10.00    --   19.03 -37.00 -90.00   98
  3  \w    -12.00  69.00   1.00   10.00    --   19.03-114.00-107.00   81
  4  \w    -92.00   6.00   1.00   10.00    --  -19.65 -37.00 120.00   98
  5  \w    -50.00  50.00   1.00   10.00    --  -19.65  77.00 120.00  100
  6  \w    -70.00  12.00   1.00   10.00    --  -19.65 114.00 -15.00   82
  7  \w    -88.00   2.00   1.00   10.00    --  -19.65 -57.00 -30.00   90
  8  \w    -88.00   2.00   1.00   10.00    --  -19.65 -57.00  60.00   90
  9  \w    -25.00  22.00   1.00   10.00    --  -19.65 -99.00 -90.00   47
 10  \w    -92.00   6.00   1.00   10.00    --  -19.65 -37.00-150.00   98
 11  \w     35.00  95.00   1.00   10.00    --   19.03 178.00 150.00   60
 12  \w    -25.00  61.00   1.00   10.00    --   19.03 -99.00 -60.00   86
 13  \w    -25.00  61.00   1.00   10.00    --   19.03 -99.00-150.00   86
 14  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00-180.00  146
 15  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00-150.00  146
 16  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00-120.00  146
 17  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00 -90.00  146
 18  \w    -25.00  22.00   1.00   10.00    --  -19.65 -99.00-180.00   47
 19  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00 -30.00  146
 20  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00   0.00  146
 21  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00  30.00  146
 22  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00  60.00  146
 23  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00  90.00  146
 24  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00 120.00  146
 25  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00 150.00  146
 26  \w    -54.00  92.00   1.00   10.00    --   19.03   0.00 -60.00  146
 27  \w    -93.00  53.00   1.00   10.00    --  -19.65   0.00-150.00  146
 28  \w    -93.00  53.00   1.00   10.00    --  -19.65   0.00-120.00  146
 29  \w    -93.00  53.00   1.00   10.00    --  -19.65   0.00 -90.00  146
 30  \w    -93.00  53.00   1.00   10.00    --  -19.65   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      -0.0535116000
_diffrn_orient_matrix_UB_12      0.0258932000
_diffrn_orient_matrix_UB_13      -0.0500104000
_diffrn_orient_matrix_UB_21      -0.0170605000
_diffrn_orient_matrix_UB_22      -0.0472312000
_diffrn_orient_matrix_UB_23      -0.0297642000
_diffrn_orient_matrix_UB_31      -0.0654155000
_diffrn_orient_matrix_UB_32      -0.0095899000
_diffrn_orient_matrix_UB_33      0.0157490000
_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  0.0784
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            49626
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.497
_diffrn_reflns_theta_min         3.466
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73292
_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    1.655
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.310
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.31(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0979P)^2^+3.9479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.876
_reflns_number_gt                3319
_reflns_number_total             3616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00881a2.cif
_cod_data_source_block           jsx04r_pl
_cod_depositor_comments
'Adding full bibliography for 7247455--7247462.cif.'
_cod_database_code               7247460
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MnC9N4H4O4
_chemical_oxdiff_usercomment     'Mn L4 4DMF 1H2O'
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.637
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.69(5)
 0.31(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H2 of C2, H13 of C13, H15 of C15, H46 of C46, H33A of
  C33A, H33B of C33B
 At 1.5 times of:
  All C(H,H,H) groups, H41 of C36, All O(H,H) groups
3. Restrained distances
 O41-H41
 1.08 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O45 \\sim C46 \\sim N47 \\sim C48 \\sim C49: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 O45, C46, N47, C48, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H42A(0.5) H42B(0.5) N32A(0.5) N32B(0.5) C48(0.5) H48A(0.5)
 H48B(0.5) H48C(0.5) C46(0.5) H46(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5)
 C33A(0.5) H33A(0.5) C33B(0.5) H33B(0.5)
7.a Riding coordinates:
 O42(H42A,H42B), C1(H1A,H1B), C21(H21A,H21B), C33B(H33B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C46(H46), C13(H13), C15(H15), C33A(H33A)
7.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              11610
_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 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.895