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_1564933
_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         'C77 H69 Cl Cu Mn3 N13 O12, 0.5(C2 H3 N)'
_chemical_formula_sum            'C78 H70.5 Cl Cu Mn3 N13.5 O12'
_chemical_formula_weight         1652.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-05
_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                90
_cell_angle_beta                 94.92(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.374(3)
_cell_length_b                   32.954(7)
_cell_length_c                   25.956(5)
_cell_measurement_reflns_used    128693
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.643
_cell_measurement_theta_min      0.787
_cell_volume                     10545(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '13.3 (Dectris Eiger detectors)'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.782
_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  0.0890
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.782
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            128693
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.643
_diffrn_reflns_theta_min         0.787
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.626
_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    1.041
_exptl_crystal_description       plate
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         21566
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.1478
_refine_ls_R_factor_gt           0.1106
_refine_ls_shift/su_max          0.001
_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          0.3192
_refine_ls_wR_factor_ref         0.3501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12327
_reflns_number_total             21566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04712d2.cif
_cod_data_source_block           test_CCDC3
_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_formula_sum        'C78 H70.50 Cl Cu Mn3 N13.50 O12'
_cod_database_code               1564933
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.906
_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, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C55-C56
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl7) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: H53A(0.25) H53B(0.25) H53C(0.25) H53D(0.25) H53E(0.25) H53F(0.25)
 H56A(0.25) H56B(0.25) H56C(0.25) H56D(0.25) H56E(0.25) H56F(0.25) N60(0.5)
 C61(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB)
5.b 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), C22D(H22D), C23D(H23D), C25D(H25D), C26D(H26D)
5.c Disordered Me refined with riding coordinates:
 C53(H53A,H53B,H53C,H53D,H53E,H53F), C56(H56A,H56B,H56C,H56D,H56E,H56F)
5.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C36A(H36A,
 H36B,H36C), C37A(H37A,H37B,H37C), C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F),
 C36B(H36D,H36E,H36F), C37B(H37D,H37E,H37F), C16C(H16G,H16H,H16I), C17C(H17G,
 H17H,H17I), C16D(H16J,H16K,H16L), C17D(H17J,H17K,H17L)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 846 electrons were 
found in a volume of 3921\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
9.5[CH3CN] per Asymmetric Unit 
which account for 836 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              70498
_shelx_hkl_checksum              37133
_shelx_fab_checksum              7617
_olex2_submission_special_instructions 'No special instructions were received'