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_1557246
_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, 3.75(C8 H10)'
_chemical_formula_sum            'C105 H103.5 Mn3 N12 O12'
_chemical_formula_weight         1890.31
_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     dual
_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                93.98(3)
_cell_angle_beta                 97.43(3)
_cell_angle_gamma                92.02(3)
_cell_formula_units_Z            2
_cell_length_a                   12.276(3)
_cell_length_b                   12.869(3)
_cell_length_c                   31.586(6)
_cell_measurement_reflns_used    50428
_cell_measurement_temperature    100(2)
_cell_volume                     4931(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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.864
_diffrn_measured_fraction_theta_max 0.658
_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     0.71076
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_Laue_measured_fraction_full 0.864
_diffrn_reflns_Laue_measured_fraction_max 0.658
_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       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            50428
_diffrn_reflns_point_group_measured_fraction_full 0.864
_diffrn_reflns_point_group_measured_fraction_max 0.658
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.099
_diffrn_reflns_theta_min         0.652
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  29.099
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       plate
_exptl_crystal_F_000             1977
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.062
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.663
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1210
_refine_ls_number_reflns         17416
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.663
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.1480
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4430
_refine_ls_wR_factor_ref         0.4652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10440
_reflns_number_total             17416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0fd00012d2.cif
_cod_data_source_block           MnMOF-1(p-xylene)
_cod_depositor_comments
'Adding full bibliography for 1557244--1557251.cif.'
_cod_original_cell_volume        4931.1(18)
_cod_original_formula_sum        'C105 H103.50 Mn3 N12 O12'
_cod_database_code               1557246
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.776
_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 planarity
 C101, C102, C103, C107
 with sigma of 0.1
3. Others
 Fixed Sof: C103(0.5) H103(0.5) C102(0.5) H102(0.5) C101(0.5) C107(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1(H1A,H1B)
4.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),
 C62(H62), C63(H63), C65(H65), C66(H66), C72(H72), C73(H73), C75(H75), C76(H76),
  C82(H82), C83(H83), C85(H85), C86(H86), C96(H96), C92(H92), C103(H103),
 C102(H102)
4.c Idealised Me refined as rotating group:
 C97(H97A,H97B,H97C), C16A(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C16(H16G,
 H16H,H16I), C17A(H17A,H17B,H17C), C17B(H17D,H17E,H17F), C17(H17G,H17H,H17I),
 C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C26(H26G,H26H,H26I), C27A(H27A,
 H27B,H27C), C27B(H27D,H27E,H27F), C27(H27G,H27H,H27I), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C87(H87A,H87B,
 H87C), C88(H88A,H88B,H88C), C107(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'