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_7247458
_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         'C9 H9 Mn N4 O5.5, 2(H O0.5)'
_chemical_formula_sum            'C9 H11 Mn N4 O6.5'
_chemical_formula_weight         334.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4647(4)
_cell_length_b                   15.9470(6)
_cell_length_c                   13.4871(3)
_cell_measurement_reflns_used    3170
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5310
_cell_measurement_theta_min      3.7100
_cell_volume                     2465.81(14)
_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      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.907
_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    -54.00  63.00   1.00   18.00    --   18.95 -19.00 -90.00  117
  2  \w    -96.00 -32.00   1.00   18.00    --  -19.50 178.00 120.00   64
  3  \w     -4.00  35.00   1.00   18.00    --   18.95  66.00  57.00   39
  4  \w     -2.00  88.00   1.00   18.00    --   18.95  57.00 -60.00   90
;
_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      -0.0463642000
_diffrn_orient_matrix_UB_12      0.0293847000
_diffrn_orient_matrix_UB_13      -0.0026824000
_diffrn_orient_matrix_UB_21      0.0076883000
_diffrn_orient_matrix_UB_22      0.0095994000
_diffrn_orient_matrix_UB_23      0.0509349000
_diffrn_orient_matrix_UB_31      0.0402178000
_diffrn_orient_matrix_UB_32      0.0319964000
_diffrn_orient_matrix_UB_33      -0.0128006000
_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  0.0492
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14713
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.185
_diffrn_reflns_theta_min         3.460
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75589
_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    1.800
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3154
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0226P)^2^+4.1163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2375
_reflns_number_total             3154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00881a2.cif
_cod_data_source_block           jsx01
_cod_depositor_comments
'Adding full bibliography for 7247455--7247462.cif.'
_cod_original_formula_sum        'C9 H11 Mn N4 O6.50'
_cod_database_code               7247458
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C9H6N4O4Mn1
_chemical_oxdiff_usercomment     'acetone wash'
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.732
_reflns_odcompleteness_completeness 99.58
_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 O(H,H,H,H,H,H) groups
2. Restrained distances
 O41-H41
 -0.95 with sigma of 0.02
 O43-H43A
 -0.95 with sigma of 0.02
 O52-H52
 -0.95 with sigma of 0.02
 O43-H43B
 0.95 with sigma of 0.02
 O42-H42
 -0.95 with sigma of 0.02
3. Others
 Fixed Sof: H43B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C33(H33), C35(H35)
;
_shelx_res_checksum              38502
_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 1.246
_oxdiff_exptl_absorpt_empirical_full_min 0.814