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_1564928
_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 Br Cu Mn3 N12 O12, 2(C6 H12)'
_chemical_formula_sum            'C87 H90 Br Cu Mn3 N12 O12'
_chemical_formula_weight         1803.97
_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             2021-03-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-07-30 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.23(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.335(3)
_cell_length_b                   33.732(7)
_cell_length_c                   13.089(3)
_cell_measurement_reflns_used    60121
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.684
_cell_measurement_theta_min      1.207
_cell_volume                     5437(2)
_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 0.873
_diffrn_measured_fraction_theta_max 0.655
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1533
_diffrn_reflns_av_unetI/netI     0.1440
_diffrn_reflns_Laue_measured_fraction_full 0.873
_diffrn_reflns_Laue_measured_fraction_max 0.655
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60121
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.655
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.684
_diffrn_reflns_theta_min         1.207
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_type   none
_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    1.102
_exptl_crystal_description       plate
_exptl_crystal_F_000             1862
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         13272
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.2891
_refine_ls_R_factor_gt           0.1624
_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          0.4192
_refine_ls_wR_factor_ref         0.4936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3153
_reflns_number_total             13272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04712d2.cif
_cod_data_source_block           test
_cod_original_cell_volume        5437.5(19)
_cod_database_code               1564928
_shelx_shelxl_version_number     2018/3
_diffrn_measurement_detector_type 'Dectris Eiger 16M'
_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
 C33-C36
 1.45 with sigma of 0.02
 C35-C37
 1.45 with sigma of 0.02
 C84-C85
 1.54 with sigma of 0.02
 C82-C83
 1.54 with sigma of 0.02
 C81-C86
 -1.5 with sigma of 0.02
 C81-C82
 -1.5 with sigma of 0.02
 C91-C92
 1.54 with sigma of 0.02
 C83-C84
 -1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: C81(0.5) H81A(0.5) H81B(0.5) C82(0.5) H82A(0.5) H82B(0.5) C83(0.5)
 H83A(0.5) H83B(0.5) C84(0.5) H84A(0.5) H84B(0.5) C85(0.5) H85A(0.5) H85B(0.5)
 C86(0.5) H86A(0.5) H86B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C51(H51A,H51B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C91(H91A,H91B), C92(H92A,H92B),
  C93(H93A,H93B)
5.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C25(H25), C26(H26), C42(H42), C43(H43), C45(H45),
 C46(H46), C72(H72), C73(H73), C75(H75), C76(H76)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1993
_shelx_hkl_checksum              70819
_shelx_fab_checksum              83944
_olex2_submission_special_instructions 'No special instructions were received'