Coordination Modulated On-Off Switching of Flexibility in a Metal-organic Framework
Albalad, jorge; Peralta, Ricardo; Huxley, Michael; Tsoukatos, Steven; Shi, Zhaolin; Zhang, Yue-Biao; Evans, Jack D.; Sumby, Christopher J.; Doonan, Christian J.; Chemical Science  (2021) –; doi:10.1039/D1SC04712D

data_1564931
_publ_section_title
;
 Coordination Modulated On-Off Switching of Flexibility in a Metal-organic
 Framework
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04712D
_journal_year                    2021
_chemical_formula_moiety         'C75 H66 Mn3 N12 O12'
_chemical_formula_sum            'C75 H66 Cl0 Cu0 Mn3 N12 O12'
_chemical_formula_weight         1492.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-30 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                96.83(3)
_cell_angle_beta                 91.48(3)
_cell_angle_gamma                90.60(3)
_cell_formula_units_Z            2
_cell_length_a                   12.341(3)
_cell_length_b                   12.924(3)
_cell_length_c                   27.121(5)
_cell_measurement_reflns_used    51874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.356
_cell_measurement_theta_min      1.587
_cell_volume                     4293.1(17)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '13.3 (Dectris Eiger detectors)'
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.673
_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  0.1806
_diffrn_reflns_av_unetI/netI     0.2144
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.673
_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       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            51874
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.673
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         29.356
_diffrn_reflns_theta_min         1.587
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       plate
_exptl_crystal_F_000             1542
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         15879
_refine_ls_number_restraints     1478
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.2557
_refine_ls_R_factor_gt           0.1789
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4393
_refine_ls_wR_factor_ref         0.5042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4230
_reflns_number_total             15879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04712d2.cif
_cod_data_source_block           test_CCDC1
_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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        4293.1(15)
_cod_database_code               1564931
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.917
_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 C(H,H,H) groups
2. Restrained distances
 C24A-C27A
 1.5 with sigma of 0.02
 C44A-C47A
 1.5 with sigma of 0.02
 C44C-C47C
 1.5 with sigma of 0.02
 C36B-C33B
 1.45 with sigma of 0.02
 N11B-C1B
 -1.36 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A \\sim C21A \\sim C22A \\sim
C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C33A \\sim C34A \\sim
C35A \\sim C36A \\sim C37A \\sim C41A \\sim C42A \\sim C43A \\sim C44A \\sim
C45A \\sim C46A \\sim C47A \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim
C17B \\sim C21B \\sim C22B \\sim C23B \\sim C24B \\sim C25B \\sim C26B \\sim
C27B \\sim C33B \\sim C34B \\sim C35B \\sim C36B \\sim C37B \\sim C41B \\sim
C42B \\sim C43B \\sim C44B \\sim C45B \\sim C46B \\sim C47B \\sim C13C \\sim
C14C \\sim C15C \\sim C16C \\sim C17C \\sim C21C \\sim C22C \\sim C23C \\sim
C24C \\sim C25C \\sim C26C \\sim C27C \\sim C33C \\sim C34C \\sim C35C \\sim
C36C \\sim C37C \\sim C41C \\sim C42C \\sim C43C \\sim C44C \\sim C45C \\sim
C46C \\sim C47C \\sim C1A \\sim C1B \\sim C1C \\sim N11A \\sim N12A \\sim N31A
\\sim N32A \\sim N11B \\sim N12B \\sim N31B \\sim N32B \\sim N11C \\sim N12C
\\sim N31C \\sim N32C \\sim O28A \\sim O29A \\sim O48A \\sim O49A \\sim O28B
\\sim O29B \\sim O48B \\sim O49B \\sim O28C \\sim O29C \\sim O48C \\sim O49C:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Mn1) \\sim Ueq, Uanis(Mn2) \\sim Ueq, Uanis(Mn3) \\sim Ueq, Uanis(Mn4)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C13A, C14A, C15A, C16A, C17A, C21A, C22A, C23A, C24A, C25A, C26A, C27A, C33A,
 C34A, C35A, C36A, C37A, C41A, C42A, C43A, C44A, C45A, C46A, C47A, C13B, C14B,
 C15B, C16B, C17B, C21B, C22B, C23B, C24B, C25B, C26B, C27B, C33B, C34B, C35B,
 C36B, C37B, C41B, C42B, C43B, C44B, C45B, C46B, C47B, C13C, C14C, C15C, C16C,
 C17C, C21C, C22C, C23C, C24C, C25C, C26C, C27C, C33C, C34C, C35C, C36C, C37C,
 C41C, C42C, C43C, C44C, C45C, C46C, C47C, C1A, C1B, C1C, N11A, N12A, N31A,
 N32A, N11B, N12B, N31B, N32B, N11C, N12C, N31C, N32C, O28A, O29A, O48A, O49A,
 O28B, O29B, O48B, O49B, O28C, O29C, O48C, O49C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB)
5.b Me refined with riding coordinates:
 C16B(H16D,H16E,H16F), C36B(H36D,H36E,H36F), C16C(H16G,H16H,H16I), C17C(H17G,
 H17H,H17I)
5.c Aromatic/amide H refined with riding coordinates:
 C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A), C42A(H42A), C43A(H43A),
 C45A(H45A), C46A(H46A), C22B(H22B), C23B(H23B), C25B(H25B), C26B(H26B),
 C42B(H42B), C43B(H43B), C45B(H45B), C46B(H46B), C22C(H22C), C23C(H23C),
 C25C(H25C), C26C(H26C), C42C(H42C), C43C(H43C), C45C(H45C), C46C(H46C)
5.d Fitted pentagon refined as free rotating group:
 N11B(N12B,C13B,C14B,C15B), N31B(N32B,C33B,C34B,C35B), N11C(N12C,C13C,C14C,
 C15C), N31C(N32C,C33C,C34C,C35C)
5.e Fitted hexagon refined as free rotating group:
 C21B(C22B,C23B,C24B,C25B,C26B), C41C(C42C,C43C,C44C,C45C,C46C)
5.f Idealised Me refined as rotating group:
 C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C36A(H36A,H36B,H36C), C37A(H37A,
 H37B,H37C), C17B(H17D,H17E,H17F), C37B(H37D,H37E,H37F), C36C(H36G,H36H,H36I),
 C37C(H37G,H37H,H37I)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 328 electrons were 
found in a volume of 1268\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
2.5[C5H12], 1[CuCl] per Asymmetric Unit 
which account for 302 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22387
_shelx_hkl_checksum              62414
_shelx_fab_checksum              18403
_olex2_submission_special_instructions 'No special instructions were received'