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_1564929
_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, 2(C7 H8)'
_chemical_formula_sum            'C89 H82 Cl Cu Mn3 N12 O12'
_chemical_formula_weight         1775.47
_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                 94.014(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3865(6)
_cell_length_b                   33.158(2)
_cell_length_c                   13.0706(6)
_cell_measurement_reflns_used    3961
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.7000
_cell_measurement_theta_min      3.5020
_cell_volume                     5355.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -11.00  89.00   1.00  110.00    --   18.87  77.00 120.00  100
  2  \w    -50.00  40.00   1.00  110.00    --   18.87 -57.00 -30.00   90
  3  \w    -11.00  89.00   1.00  110.00    --   18.87  77.00   0.00  100
  4  \w     35.00  95.00   1.00  110.00    --   18.87 178.00-120.00   60
  5  \w    -25.00  22.00   1.00  110.00    --  -19.50 -99.00-120.00   47
  6  \w    -41.00  49.00   1.00  110.00    --  -19.50  57.00 -90.00   90
  7  \w    -45.00  53.00   1.00  110.00    --  -19.50  37.00  90.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0155487000
_diffrn_orient_matrix_UB_12      0.0201698000
_diffrn_orient_matrix_UB_13      -0.0116153000
_diffrn_orient_matrix_UB_21      -0.0056496000
_diffrn_orient_matrix_UB_22      -0.0049069000
_diffrn_orient_matrix_UB_23      -0.0529360000
_diffrn_orient_matrix_UB_31      -0.0549504000
_diffrn_orient_matrix_UB_32      -0.0051840000
_diffrn_orient_matrix_UB_33      0.0047736000
_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  0.1769
_diffrn_reflns_av_unetI/netI     0.2280
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            63186
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.383
_diffrn_reflns_theta_min         3.354
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.101
_exptl_crystal_description       plate
_exptl_crystal_F_000             1834
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.451
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         13398
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1897
_refine_ls_R_factor_gt           0.0999
_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^)+(0.1351P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2585
_refine_ls_wR_factor_ref         0.3044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6039
_reflns_number_total             13398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04712d2.cif
_cod_data_source_block           cucl_tol_(good)
_cod_database_code               1564929
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H30N4O4Mn3Cu1
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C81-C87
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C51 \\sim N61 \\sim N62 \\sim C63 \\sim C64 \\sim C65: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C51) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C81, C82, C83, C84, C85, C86, C87
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, N61, N62, C63, C64, C65
 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 Me refined with riding coordinates:
 C87(H87A,H87B,H87C)
5.c 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), C82(H82), C83(H83), C84(H84),
  C85(H85), C86(H86)
5.d 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_special_details
;
A solvent mask was calculated and 100 electrons were 
found in a volume of 1794\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
2[C7H8], 2[C7H8] per Asymmetric Unit 
which account for 400 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87373
_shelx_hkl_checksum              3267
_shelx_fab_checksum              97730
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.161
_oxdiff_exptl_absorpt_empirical_full_min 0.858