Probing post-synthetic metallation in metal-organic frameworks: insights from X-ray crystallography.
Bloch, Witold M.; Burgun, Alexandre; Doonan, Christian J.; Sumby, Christopher J.; Chemical communications (Cambridge, England) 51 (2015) 5486–5489; doi:10.1039/c4cc09639h

data_7116950
_publ_section_title
;
 Probing post-synthetic metallation in metal-organic frameworks: insights
 from X-ray crystallography.
;
_journal_issue                   25
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5486
_journal_page_last               5489
_journal_paper_doi               10.1039/c4cc09639h
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C77 H69 Cl5.25 Mn5.5 N13 O16.5'
_chemical_formula_weight         1928.73
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-12-02 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.45(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.338(3)
_cell_length_b                   33.330(7)
_cell_length_c                   25.857(5)
_cell_measurement_temperature    100(2)
_cell_volume                     10543(4)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.853
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            200686
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         31.392
_diffrn_reflns_theta_min         0.794
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       plate
_exptl_crystal_F_000             3923
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
The SQUEEZE routine of PLATON was applied to the collected data, which 
resulted in significant reductions in R1 and wR2 and an improvement 
in the GOF. R1, wR2 and GOF before SQUEEZE routine: 17.35%, 51.41%, 
2.242; after SQUEEZE routine: 11.89%, 32.77%, 1.020. The exact nature 
of the species in the solvent accessible region calculated from the 
result of SQUEEZE routine could not be determined due to uncertainties 
in the form of the additional anion (Cl- vs MnCl42-).
;
_refine_diff_density_max         2.191
_refine_diff_density_min         -3.379
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1158
_refine_ls_number_reflns         30063
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.1187
_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^)+(0.1633P)^2^+55.9433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3126
_refine_ls_wR_factor_ref         0.3259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23088
_reflns_number_total             30063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc09639h2.cif
_cod_data_source_block           1MnCH3CN
_cod_original_formula_sum        'C77 H69 Cl5.25 Mn5.50 N13 O16.50'
_cod_database_code               7116950
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2013-4
_shelx_res_checksum              38226
_shelx_hkl_checksum              50741