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_1557248
_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         'C75 H66 Mn3 N12 O12, 2(C4 H10 O)'
_chemical_formula_sum            'C97 H126 Mn3 N12 O18'
_chemical_formula_weight         1912.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                99.40(3)
_cell_angle_beta                 97.35(3)
_cell_angle_gamma                91.57(3)
_cell_formula_units_Z            2
_cell_length_a                   12.364(3)
_cell_length_b                   12.947(3)
_cell_length_c                   30.366(6)
_cell_measurement_reflns_used    53314
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.162
_cell_measurement_theta_min      0.686
_cell_volume                     4750.4(19)
_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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.880
_diffrn_measured_fraction_theta_max 0.665
_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     0.7107
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.880
_diffrn_reflns_Laue_measured_fraction_max 0.665
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            53314
_diffrn_reflns_point_group_measured_fraction_full 0.880
_diffrn_reflns_point_group_measured_fraction_max 0.665
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.162
_diffrn_reflns_theta_min         0.686
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             2022
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
                          ?
The structure contains solvent accessible voids that contain diethyl 
ether. To account for the removed electron density, 4 diethyl 
ether molecules (42e) per asymmetric unit were added to the formula. 
Two diethyl ether molecules were located in the difference map and refined 
giving a total of 6.
;
_refine_diff_density_max         1.623
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.437
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         17030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.437
_refine_ls_R_factor_all          0.2500
_refine_ls_R_factor_gt           0.2135
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5779
_refine_ls_wR_factor_ref         0.5982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10111
_reflns_number_total             17030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0fd00012d2.cif
_cod_data_source_block           MnMOF-1(DEE)
_cod_depositor_comments
'Adding full bibliography for 1557244--1557251.cif.'
_cod_original_cell_volume        4750.4(17)
_cod_database_code               1557248
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.736
_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.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C61(H61A,H61B), C63(H63A,
 H63B), C66(H66A,H66B), C68(H68A,H68B)
2.b Aromatic/amide H refined with riding coordinates:
 C32A(H32A), C32B(H32B), C32C(H32C), C33A(H33A), C33B(H33B), C33C(H33C),
 C35A(H35A), C35B(H35B), C35C(H35C), C36A(H36A), C36B(H36B), C36C(H36C),
 C42A(H42A), C42B(H42B), C42C(H42C), C43A(H43A), C43B(H43B), C43C(H43C),
 C45A(H45A), C45B(H45B), C45C(H45C), C46A(H46A), C46B(H46B), C46C(H46C)
2.c Idealised Me refined as rotating group:
 C16A(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C16C(H16G,H16H,H16I), C17A(H17A,
 H17B,H17C), C17B(H17D,H17E,H17F), C17C(H17G,H17H,H17I), C26A(H26A,H26B,H26C),
 C26B(H26D,H26E,H26F), C26C(H26G,H26H,H26I), C27A(H27A,H27B,H27C), C27B(H27D,
 H27E,H27F), C27C(H27G,H27H,H27I), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C69(H69A,H69B,H69C)
;
_olex2_submission_special_instructions 'No special instructions were received'