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_1564932
_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 Cl Cu Mn3 N12 O12'
_chemical_formula_sum            'C75 H66 Cl Cu Mn3 N12 O12'
_chemical_formula_weight         1591.20
_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                94.70(3)
_cell_angle_beta                 95.44(3)
_cell_angle_gamma                92.66(3)
_cell_formula_units_Z            2
_cell_length_a                   12.308(3)
_cell_length_b                   12.898(3)
_cell_length_c                   30.822(6)
_cell_measurement_reflns_used    51592
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.721
_cell_measurement_theta_min      1.332
_cell_volume                     4847.3(19)
_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 0.897
_diffrn_measured_fraction_theta_max 0.682
_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  0.1554
_diffrn_reflns_av_unetI/netI     0.1757
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.682
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            51592
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.682
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         28.721
_diffrn_reflns_theta_min         1.332
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.679
_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    1.090
_exptl_crystal_description       plate
_exptl_crystal_F_000             1634
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.932
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         17139
_refine_ls_number_restraints     254
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.2104
_refine_ls_R_factor_gt           0.1375
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3446
_refine_ls_wR_factor_ref         0.4077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5928
_reflns_number_total             17139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04712d2.cif
_cod_data_source_block           test_CCDC2
_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        4847.3(17)
_cod_database_code               1564932
_shelx_shelxl_version_number     2018/3
_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
 C35B-C37B
 1.45 with sigma of 0.02
 C33B-C36B
 1.45 with sigma of 0.02
 C15B-C17B
 1.45 with sigma of 0.02
 C13B-C16B
 1.45 with sigma of 0.02
 C1B-N31B
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1B \\sim N11B \\sim N12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim
C17B \\sim C21B \\sim N31B \\sim N32B \\sim C33B \\sim C34B \\sim C35B \\sim
C36B \\sim C37B \\sim C41B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C1B, N11B, N12B, C13B, C14B, C15B, C16B, C17B, C21B, N31B, N32B, C33B, C34B,
 C35B, C36B, C37B, C41B
 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)
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 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), C36B(H36D,H36E,H36F), C37B(H37D,H37E,H37F),
 C16C(H16G,H16H,H16I), C17C(H17G,H17H,H17I), C36C(H36G,H36H,H36I), C37C(H37G,
 H37H,H37I)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 310 electrons were 
found in a volume of 1870\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3.75[C4H10O] per Asymmetric Unit 
which account for 315 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26247
_shelx_hkl_checksum              42700
_shelx_fab_checksum              13460
_olex2_submission_special_instructions 'No special instructions were received'