Capturing snapshots of post-synthetic metallation chemistry in metal-organic frameworks
Witold M. Bloch; Alexandre Burgun; Campbell J. Coghlan; Richmond Lee; Michelle L. Coote; Christian J. Doonan; Christopher J. Sumby; Nature Chemistry 6 (2014) 906–912; doi:10.1038/nchem.2045

data_1551927
_publ_section_title
;
 Capturing snapshots of post-synthetic metallation chemistry in
 metal-organic frameworks
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              906
_journal_page_last               912
_journal_paper_doi               10.1038/nchem.2045
_journal_volume                  6
_journal_year                    2014
_chemical_formula_sum            'C75 H66 Mn3 N12 O16'
_chemical_formula_weight         1556.22
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 100.629(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9293(10)
_cell_length_b                   18.4694(7)
_cell_length_c                   28.346(2)
_cell_measurement_reflns_used    4139
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.9604
_cell_measurement_theta_min      2.5511
_cell_volume                     8711.0(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'X-Seed (Barbour, 2003)'
_computing_publication_material  'CIFTAB (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1695
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.756
_diffrn_measurement_details
;
  1 omega  -25.00   12.00   1.0000  205.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7025  110.0000  -15.0000 37

  2 omega   43.00   84.00   1.0000  205.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7025  179.0000 -180.0000 41

  3 omega  -90.00   31.00   1.0000  205.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5619    0.0000   90.0000 121

  4 omega  -51.00   39.00   1.0000  205.0000
omega____ theta____ kappa____ phi______ frames
    -       17.7025  -57.0000 -150.0000 90

  5 omega  -43.00    3.00   1.0000  205.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5619  -57.0000   60.0000 46

  6 omega  -55.00  -38.00   1.0000  205.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5619  110.0000  -69.0000 17

;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1103
_diffrn_reflns_av_sigmaI/netI    0.1677
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            27623
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3212
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         9635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.1272
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+135.7931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2276
_refine_ls_wR_factor_ref         0.2533
_reflns_number_gt                6062
_reflns_number_total             9635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2045-s2.cif
_cod_data_source_block           1-des
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1551927