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_7247456
_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         'C10.5 H9 Mn0.5 N2 O3'
_chemical_formula_sum            'C10.5 H9 Mn0.5 N2 O3'
_chemical_formula_weight         238.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-23
_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                 101.761(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.3665(10)
_cell_length_b                   4.5514(2)
_cell_length_c                   21.1136(9)
_cell_measurement_reflns_used    2525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6730
_cell_measurement_theta_min      4.2630
_cell_volume                     1916.06(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.955
_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     33.00  67.00   0.50    0.07    --  104.72 -57.00-180.00   68
  2  \w     33.00  67.00   0.50    0.07    --  104.72 -57.00-120.00   68
  3  \w     33.00  67.00   0.50    0.07    --  104.72 -57.00  30.00   68
  4  \w     33.00  67.00   0.50    0.07    --  104.72 -57.00  60.00   68
  5  \w    -24.00  35.00   0.50    0.05    --   48.77 -34.00 147.00  118
  6  \w    -25.00  16.00   0.50    0.05    --   48.77 -19.00  30.00   82
  7  \w     39.00 121.00   0.50    0.05    --   48.77  38.00  30.00  164
  8  \w     94.00 178.00   0.50    0.07    --  104.72  19.00   0.00  168
  9  \w     94.00 178.00   0.50    0.07    --  104.72  34.00 -54.00  168
 10  \w     39.00 123.00   0.50    0.05    --   48.77  34.00 -54.00  168
 11  \w    -16.00  26.00   0.50    0.05    --  -48.77  19.00  90.00   84
 12  \w    -67.00 -18.00   0.50    0.07    --  -90.00  57.00 120.00   98
 13  \w    -67.00 -18.00   0.50    0.07    --  -90.00  57.00 -90.00   98
 14  \w    -35.00  25.00   0.50    0.05    --  -48.77  34.00 -54.00  120
 15  \w     34.00 111.00   0.50    0.07    --  104.72-125.00  90.00  154
 16  \w     34.00 111.00   0.50    0.07    --  104.72-125.00 150.00  154
 17  \w   -121.00 -39.00   0.50    0.05    --  -48.77 -38.00  60.00  164
 18  \w   -122.00 -39.00   0.50    0.05    --  -48.77 -34.00 147.00  166
 19  \w   -121.00 -90.00   0.50    0.05    --  -48.77 -38.00   0.00   62
 20  \w   -121.00 -39.00   0.50    0.05    --  -48.77 -38.00-150.00  164
 21  \w   -161.00-110.00   0.50    0.07    --  -90.00 -77.00-120.00  102
 22  \w   -161.00-103.00   0.50    0.07    --  -90.00 -57.00  90.00  116
 23  \w   -163.00 -79.00   0.50    0.07    --  -90.00 -34.00 147.00  168
 24  \w   -121.00 -94.00   0.50    0.05    --  -48.77-125.00 120.00   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      -0.0317972000
_diffrn_orient_matrix_UB_12      -0.1021311000
_diffrn_orient_matrix_UB_13      0.0564948000
_diffrn_orient_matrix_UB_21      -0.0623149000
_diffrn_orient_matrix_UB_22      -0.1080909000
_diffrn_orient_matrix_UB_23      -0.0485734000
_diffrn_orient_matrix_UB_31      0.0328256000
_diffrn_orient_matrix_UB_32      -0.3040450000
_diffrn_orient_matrix_UB_33      -0.0016975000
_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  0.0879
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9310
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.296
_diffrn_reflns_theta_min         4.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52822
_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 brownish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       plate
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1922
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0472P)^2^+4.3852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1358
_reflns_number_total             1922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00881a2.cif
_cod_data_source_block           mn_l2_petal-100k_2_auto
_cod_depositor_comments
'Adding full bibliography for 7247455--7247462.cif.'
_cod_original_formula_sum        'C10.50 H9 Mn0.50 N2 O3'
_cod_database_code               7247456
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MnC10H10O4N4
_chemical_oxdiff_usercomment     '24Mn27L24DMF2H2O_24h_white_flower in corner'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 O(H,H) groups
2. Restrained distances
 O17-H17A = O17-H17B
 0.87 with sigma of 0.02
 H17A-H17B
 1.38 with sigma of 0.04
 Mn1-H17A \\sim Mn1-H17B
 with sigma of 0.02
3. Others
 Fixed Sof: H13A(0.5) H13B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C4(H4), C3(H3), C12(H12), C6(H6), C7(H7)
;
_shelx_res_checksum              83910
_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 1.574
_oxdiff_exptl_absorpt_empirical_full_min 0.763