MOF matrix isolation: cooperative conformational mobility enables reliable single crystal transformations.
Peralta, Ricardo A.; Huxley, Michael T.; Young, Rosemary J.; Linder-Patton, Oliver M; Evans, Jack D.; Doonan, Christian J.; Sumby, Christopher J.; Faraday discussions 225 (2021) 84–99; doi:10.1039/d0fd00012d

data_1557244
_publ_section_title
;
 MOF matrix isolation: cooperative conformational mobility enables
 reliable single crystal transformations.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              84
_journal_page_last               99
_journal_paper_doi               10.1039/d0fd00012d
_journal_volume                  225
_journal_year                    2021
_chemical_formula_moiety         '0.5(C150 H132 Mn6 N24 O24)'
_chemical_formula_sum            'C90 H126 Mn3 N12 O27'
_chemical_formula_weight         1972.84
_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     direct
_audit_creation_date             2020-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-15 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.58(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.323(3)
_cell_length_b                   32.145(6)
_cell_length_c                   12.931(3)
_cell_measurement_reflns_used    64425
_cell_measurement_temperature    100(2)
_cell_volume                     5112(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.718
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71092
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.718
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            64425
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.718
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.188
_diffrn_reflns_theta_min         1.267
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  29.188
_exptl_absorpt_correction_T_min  1.267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             2082
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;                       
The structure contains solvent accessible voids that contain methanol. 
To account for the removed electron density, 15 methanol molecules (18e)
 per asymmetric unit were added to the formula.
;
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         10099
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1272P)^2^+0.7143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.1983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8010
_reflns_number_total             10099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0fd00012d2.cif
_cod_data_source_block           test_sqd
_cod_depositor_comments
'Adding full bibliography for 1557244--1557251.cif.'
_cod_original_cell_volume        5112.3(18)
_cod_database_code               1557244
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.762
_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. Shared sites
{C1B, C1C}
3. Restrained distances
 C14B-C21B
 1.5 with sigma of 0.02
 C14C-C21C
 1.5 with sigma of 0.02
 C24B-C25B
 1.35 with sigma of 0.02
 C21B-C26B
 1.35 with sigma of 0.02
 C25B-C26B
 1.35 with sigma of 0.02
 C24C-C25C
 1.35 with sigma of 0.02
 C21C-C26C
 1.35 with sigma of 0.02
4. Restrained planarity
 C14B, C21B, C22B, C23B, C24B, C25B, C26B, C27B
 with sigma of 0.1
 N11C, N12C, C13C, C14C, C15C, C16C, C17C
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
N11B \\sim N12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim C17B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
N11C \\sim N12C \\sim C13C \\sim C14C \\sim C15C \\sim C16C \\sim C17C: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1B) = Uanis(C1C)
Uanis(C24B) = Uanis(C24C)
Uanis(C25B) = Uanis(C25C)
6. Same fragment restrains
{N11A, N12A, C13A, C14A, C15A, C16A, C17A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N11B, N12B, C13B, C14B, C15B, C16B, C17B}
{N11A, N12A, C13A, C14A, C15A, C16A, C17A} sigma for 1-2: 0.02, 1-3: 0.04
as
{N11C, N12C, C13C, C14C, C15C, C16C, C17C}
7. Others
 Sof(N11C)=Sof(N12C)=Sof(C13C)=Sof(C14C)=Sof(C15C)=Sof(C16C)=Sof(H16G)=
 Sof(H16H)=Sof(H16I)=Sof(C17C)=Sof(H17G)=Sof(H17H)=Sof(H17I)=Sof(C21C)=
 Sof(C22C)=Sof(H22C)=Sof(C23C)=Sof(H23C)=Sof(C24C)=Sof(C25C)=Sof(H25C)=
 Sof(C26C)=Sof(H26E)=1-FVAR(1)
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=0.5*(1-FVAR(2))
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=0.5*FVAR(2)
 Sof(N11B)=Sof(N12B)=Sof(C13B)=Sof(C14B)=Sof(C15B)=Sof(C16B)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C21B)=
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(C25B)=Sof(H25B)=
 Sof(C26B)=Sof(H26D)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB)
8.b Aromatic/amide H refined with riding coordinates:
 C32A(H32A), C33A(H33A), C35A(H35A), C36A(H36A), C42A(H42A), C43A(H43A),
 C45A(H45A), C46A(H46A), C22B(H22B), C23B(H23B), C25B(H25B), C26B(H26D),
 C22C(H22C), C23C(H23C), C25C(H25C), C26C(H26E)
8.c Idealised Me refined as rotating group:
 C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C26A(H26A,H26B,H26C), C27A(H27A,
 H27B,H27C), C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C16C(H16G,H16H,H16I),
 C17C(H17G,H17H,H17I)
;
_olex2_submission_special_instructions 'No special instructions were received'