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_7116951
_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            'C37.5 H33 Cl Mn2 N6 O7.5'
_chemical_formula_weight         833.03
_chemical_name_systematic        ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_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                 97.63(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.355(3)
_cell_length_b                   33.452(7)
_cell_length_c                   12.952(3)
_cell_measurement_temperature    100(2)
_cell_volume                     5306(2)
_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 0.941
_diffrn_measured_fraction_theta_max 0.939
_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  0.0674
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            85469
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.284
_diffrn_reflns_theta_min         1.663
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_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: 15.02%, 43.73%, 1.822; after SQUEEZE routine: 8.90%, 
26.36%, 1.029. The contents of the solvent region calculated from the 
result of SQUEEZE routine equates to 9 ethanol molecules.
;
_refine_diff_density_max         1.012
_refine_diff_density_min         -1.940
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.032(2)
_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   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         11393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0890
_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          0.2462
_refine_ls_wR_factor_ref         0.2636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8389
_reflns_number_total             11393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc09639h2.cif
_cod_data_source_block           1_MnCl2_EtOH
_cod_depositor_comments
;
 Removing data item '_space_group_name' since it had a mispelt data name
 and contained no additional information that was not already in the file.

 Antanas Vaitkus,
 2017-03-02

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5305.6(19)
_cod_original_formula_sum        'C37.50 H33 Cl Mn2 N6 O7.50'
_cod_database_code               7116951
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.978
_shelxl_version_number           2013-4
_shelx_res_checksum              60043
_shelx_hkl_checksum              36517