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_1564927
_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 Cu I Mn3 N12 O12'
_chemical_formula_sum            'C75 H66 Cu I Mn3 N12 O12'
_chemical_formula_weight         1682.65
_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             2021-02-27
_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                 94.47(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.334(2)
_cell_length_b                   34.440(8)
_cell_length_c                   13.084(2)
_cell_measurement_reflns_used    438
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.8690
_cell_measurement_theta_min      3.5480
_cell_volume                     5541.0(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.795
_diffrn_measurement_details
;
  1 omega  -21.00   73.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       16.0830   19.0000  -60.0000 94

  2 omega  -22.00    9.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.5517  -99.0000   60.0000 31

  3 omega  -42.00   19.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.5517   37.0000   60.0000 61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0113669000
_diffrn_orient_matrix_UB_12      -0.0201634000
_diffrn_orient_matrix_UB_13      -0.0024374000
_diffrn_orient_matrix_UB_21      -0.0457639000
_diffrn_orient_matrix_UB_22      0.0029396000
_diffrn_orient_matrix_UB_23      0.0287922000
_diffrn_orient_matrix_UB_31      -0.0331926000
_diffrn_orient_matrix_UB_32      0.0028939000
_diffrn_orient_matrix_UB_33      -0.0461200000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3740
_diffrn_reflns_av_unetI/netI     0.9529
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19217
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.139
_diffrn_reflns_theta_min         3.313
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.009
_exptl_crystal_description       plate
_exptl_crystal_F_000             1706
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.786
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         10966
_refine_ls_number_restraints     494
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.5056
_refine_ls_R_factor_gt           0.1917
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1896P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4391
_refine_ls_wR_factor_ref         0.5919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1682
_reflns_number_total             10966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04712d2.cif
_cod_data_source_block           cucl_nai_cyclohexane
_cod_original_cell_volume        5541(2)
_cod_database_code               1564927
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H30N4O4Cu1
_reflns_odcompleteness_completeness 96.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.01
_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
 C65-C67
 1.45 with sigma of 0.02
 C74-C77
 1.45 with sigma of 0.02
 C44-C47
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C21 \\sim C22 \\sim
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C33 \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim
C47 \\sim C51 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C71 \\sim
C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim N11 \\sim N12 \\sim
N31 \\sim N32 \\sim N61 \\sim N62 \\sim O28 \\sim O29 \\sim O48 \\sim O49 \\sim
O78 \\sim O79: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C13) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C1, C13, C14, C15, C16, C17, C21, C22, C23, C24, C25, C26, C27, C33, C34, C35,
  C36, C37, C41, C42, C43, C44, C45, C46, C47, C51, C63, C64, C65, C66, C67,
 C71, C72, C73, C74, C75, C76, C77, N11, N12, N31, N32, N61, N62, O28, O29, O48,
  O49, O78, O79
 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:
 C1(H1A,H1B), C51(H51A,H51B)
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              38188
_shelx_hkl_checksum              71396
_shelx_fab_checksum              73568
_olex2_submission_special_instructions 'No special instructions were received'