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_1557249
_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            'C93 H120 Mn3 N12 O21'
_chemical_formula_weight         1906.82
_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                 95.51(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.274(3)
_cell_length_b                   32.826(7)
_cell_length_c                   12.930(3)
_cell_measurement_reflns_used    67817
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.219
_cell_measurement_theta_min      1.582
_cell_volume                     5186(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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.723
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.723
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            67817
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.723
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.219
_diffrn_reflns_theta_min         1.582
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       plate
_exptl_crystal_F_000             2010
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The structure contains solvent accessible voids that contain ethanol. 
To account for the removed electron density, 9 ethanol molecules (26e) per 
asymmetric unit were added to the formula. 
;
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         10346
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0956P)^2^+1.0886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9087
_reflns_number_total             10346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0fd00012d2.cif
_cod_data_source_block           MnMOF-1(EtOH)
_cod_depositor_comments
'Adding full bibliography for 1557244--1557251.cif.'
_cod_original_cell_volume        5185.5(18)
_cod_database_code               1557249
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.753
_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(C24B) \\sim Ueq, Uanis(C24C) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
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'