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_7116949
_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            'C75 H63 Mn3 N12 O12'
_chemical_formula_weight         1489.19
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                94.65(3)
_cell_angle_beta                 93.93(3)
_cell_angle_gamma                92.40(3)
_cell_formula_units_Z            2
_cell_length_a                   12.281(3)
_cell_length_b                   12.919(3)
_cell_length_c                   30.425(6)
_cell_measurement_temperature    100(2)
_cell_volume                     4794.5(19)
_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 0.936
_diffrn_measured_fraction_theta_max 0.917
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            81801
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.918
_diffrn_reflns_theta_min         1.346
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.957
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
The structure has large solvent accessible voids. These contained 
a number of diffuse electron density peaks that could not be 
adequately identified and refined as solvent. 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: 14.81%, 45.17%, 1.757; 
after SQUEEZE routine: 5.85%, 15.63%, 0.964. The contents of the 
solvent region calculated from the result of SQUEEZE routine equates 
to 11 acetonitrile molecules.
;
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0051(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         21017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0958P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14042
_reflns_number_total             21017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc09639h2.cif
_cod_data_source_block           1_CH3CN
_cod_database_code               7116949
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2013-4
_shelx_res_checksum              22162
_shelx_hkl_checksum              13695