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_7247457
_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 H20 Mn2 N9 O11, 0.5(C6 H14 N2 O2), H2 O'
_chemical_formula_sum            'C24 H29 Mn2 N10 O13'
_chemical_formula_weight         775.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-31
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1459(3)
_cell_length_b                   12.0673(2)
_cell_length_c                   12.5517(2)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3120
_cell_measurement_theta_min      3.9870
_cell_volume                     3354.33(9)
_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 2018/2 (Sheldrick, 2018)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.877
_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     35.00 111.00   0.50    1.97    --  106.92-124.00 120.00  152
  2  \w     38.00 104.00   0.50    1.97    --  106.92-125.00 -90.00  132
  3  \w    -16.00  26.00   0.50    0.49    --  -48.77  19.00-120.00   84
  4  \w    -16.00  26.00   0.50    0.49    --  -48.77  19.00-150.00   84
  5  \w    -79.00 -18.00   0.50    1.97    --  -90.00  89.00 -49.00  122
  6  \w    -86.00 -16.00   0.50    0.49    --  -48.77 125.00  90.00  140
  7  \w   -163.00 -79.00   0.50    1.97    --  -90.00 -34.00 -18.00  168
  8  \w   -121.00 -94.00   0.50    0.49    --  -48.77-125.00-180.00   54
  9  \w   -161.00-106.00   0.50    1.97    --  -90.00 -99.00 -90.00  110
 10  \w   -121.00 -58.00   0.50    0.49    --  -48.77-147.00 -44.00  126
 11  \w   -121.00 -94.00   0.50    0.49    --  -48.77-125.00 150.00   54
 12  \w     35.00  67.00   0.50    1.97    --  106.92 -57.00 -90.00   64
 13  \w     37.00  63.00   0.50    1.97    --  106.92 -57.00-120.00   52
 14  \w     35.00  67.00   0.50    1.97    --  106.92 -57.00  90.00   64
 15  \w     35.00  67.00   0.50    1.97    --  106.92 -57.00 120.00   64
;
_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      -0.0156239000
_diffrn_orient_matrix_UB_12      -0.0334751000
_diffrn_orient_matrix_UB_13      0.1193599000
_diffrn_orient_matrix_UB_21      -0.0259373000
_diffrn_orient_matrix_UB_22      -0.1059151000
_diffrn_orient_matrix_UB_23      -0.0436000000
_diffrn_orient_matrix_UB_31      0.0626415000
_diffrn_orient_matrix_UB_32      -0.0522485000
_diffrn_orient_matrix_UB_33      0.0118507000
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17426
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         89.640
_diffrn_reflns_theta_min         3.992
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.804
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73533
_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    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.087
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.912
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3530
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0876
_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^)+(0.0591P)^2^+31.8420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2234
_refine_ls_wR_factor_ref         0.2242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3405
_reflns_number_total             3530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00881a2.cif
_cod_data_source_block           mn_l11_cube_auto_pl
_cod_depositor_comments
'Adding full bibliography for 7247455--7247462.cif.'
_cod_database_code               7247457
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Mn2C20H20O8N8
_chemical_oxdiff_usercomment     'big cube 2DMF 1.5H2O 6h 100C front of oven'
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.589
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H3A,H3B} of O3
 At 1.5 times of:
  All C(H,H,H) groups, {H1A,H1B} of O1, All O(H) groups
2. Restrained distances
 N45-C47
 1.54 with sigma of 0.02
 N45-C46
 1.54 with sigma of 0.02
3. Restrained planarity
 C47, C46, N45, C44, O43
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C47 \\sim C46 \\sim N45 \\sim C44 \\sim O43: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O39 \\sim C40 \\sim N41 \\sim C41 \\sim C42: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(N45) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C47, C46, N45, C44, O43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O39, C40, N41, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H38(0.5) H41B(0.5) H41C(0.5) H44(0.5) O1(0.5)
 H1A(0.5) H1B(0.5) N45(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) H47A(0.5)
 H47B(0.5) H47C(0.5) H42B(0.5) H42C(0.5)
7.a Riding coordinates:
 C9(H9), C10(H10)
7.b Free rotating group:
 O1(H1A,H1B)
7.c Rotating group:
 O38(H38)
7.d Secondary CH2 refined with riding coordinates:
 O3(H3A,H3B)
7.e Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C42(H42A,H42B,
 H42C)
7.f Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C12(H12), C40(H40), C44(H44), C14(H14)
;
_shelx_res_checksum              40527
_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 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.809