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_7247459
_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 H10 Mn N4 O6'
_chemical_formula_sum            'C9 H10 Mn N4 O6'
_chemical_formula_weight         325.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                 105.64(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.414(3)
_cell_length_b                   10.480(2)
_cell_length_c                   7.7400(15)
_cell_measurement_reflns_used    6611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.541
_cell_measurement_theta_min      2.435
_cell_volume                     1125.9(4)
_computing_cell_refinement       'AS QEGUI'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_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_temperature      100(2)
_diffrn_detector_area_resol_mean '13.3 (Dectris Eiger detectors)'
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.733
_diffrn_measurement_device_type
;
N. P. Cowieson, D. Aragao, M. Clift, D. J. Ericsson, C. Gee, 
S. J. Harrop, N. Mudie, S. Panjikar, J. R. Price, A. Riboldi-
Tunnicliffe, R. Williamson and T. Caradoc-Davies, MX1: a 
bending-magnet crystallography beamline serving both chemical 
and macromolecular crystallography communities at the 
Australian Synchrotron, J. Synchrotron Rad. (2015). 22, 187-190.
;
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.918
_diffrn_reflns_Laue_measured_fraction_max 0.733
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6611
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.705
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.541
_diffrn_reflns_theta_min         2.435
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 701 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2017
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0804P)^2^+4.7391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.1761
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.872
_reflns_Friedel_fraction_max     0.677
_reflns_number_gt                1721
_reflns_number_total             2017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00881a2.cif
_cod_data_source_block           cc
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7247455--7247462.cif.
;
_cod_database_code               7247459
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.889
_diffrn_measurement_detector_type 'Dectris Eiger2 9M'
_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
 Mn1A-H31A \\sim Mn1A-H31B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N21A \\sim N22A \\sim C23A \\sim C24A \\sim C25A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N21B \\sim N22B \\sim C23B \\sim C24B \\sim C25B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N11A \\sim N12A \\sim C13A \\sim C14A \\sim C15A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N11B \\sim N12B \\sim C13B \\sim C14B \\sim C15B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(O31A) \\sim Ueq, Uanis(C23A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(N21A) = Uanis(N21B)
Uanis(C24A) = Uanis(C24B)
Uanis(N11A) = Uanis(N11B)
Uanis(C1A) = Uanis(C1B)
Uanis(C14A) = Uanis(C14B)
4. Rigid body (RIGU) restrains
 N21A, N22A, C23A, C24A, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N21B, N22B, C23B, C24B, C25B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N11A, N12A, C13A, C14A, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N11B, N12B, C13B, C14B, C15B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Mn1B)=Sof(N11B)=Sof(N12B)=Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(C15B)=
 Sof(H15B)=Sof(O32B)=Sof(H32A)=Sof(H32B)=Sof(O31B)=Sof(H31C)=Sof(H31D)=
 Sof(C24B)=Sof(C25B)=Sof(H25B)=Sof(N21B)=Sof(N22B)=Sof(C23B)=Sof(H23B)=Sof(C1B)=
 Sof(H1BA)=Sof(H1BB)=1-FVAR(1)
 Sof(Mn1A)=Sof(N21A)=Sof(C25A)=Sof(H25A)=Sof(C24A)=Sof(C23A)=Sof(H23A)=
 Sof(N22A)=Sof(O31A)=Sof(H31A)=Sof(H31B)=Sof(O30A)=Sof(H30A)=Sof(H30B)=
 Sof(C14A)=Sof(C13A)=Sof(H13A)=Sof(N12A)=Sof(N11A)=Sof(C15A)=Sof(H15A)=Sof(C1A)=
 Sof(H1AA)=Sof(H1AB)=FVAR(1)
6.a Free rotating group:
 O31A(H31A,H31B)
6.b Rotating group:
 O30A(H30A,H30B), O32B(H32A,H32B), O31B(H31C,H31D)
6.c Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB)
6.d Aromatic/amide H refined with riding coordinates:
 C25A(H25A), C23A(H23A), C13A(H13A), C15A(H15A), C13B(H13B), C15B(H15B),
 C25B(H25B), C23B(H23B)
6.e Fitted pentagon refined as free rotating group:
 N21A(C25A,C24A,C23A,N22A), C14A(C13A,N12A,N11A,C15A), N11B(N12B,C13B,C14B,
 C15B), C24B(C25B,N21B,N22B,C23B)
;
_shelx_res_checksum              42261
_olex2_submission_special_instructions 'No special instructions were received'