Protecting-Group-Free Site-Selective Reactions in a Metal-Organic Framework Reaction Vessel.
Huxley, Michael T.; Burgun, Alexandre; Ghodrati, Hanieh; Coghlan, Campbell J.; Lemieux, Anthony; Champness, Neil R.; Huang, David M.; Doonan, Christian J.; Sumby, Christopher J.; Journal of the American Chemical Society 140 (2018) 6416–6425; doi:10.1021/jacs.8b02896

data_4132310
_publ_section_title
;
 Protecting-Group-Free Site-Selective Reactions in a Metal-Organic
 Framework Reaction Vessel.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6416
_journal_page_last               6425
_journal_paper_doi               10.1021/jacs.8b02896
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C45 H52 Br0.5 Mn2 N6 O11'
_chemical_formula_weight         1002.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 99.101(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3848(17)
_cell_length_b                   33.886(5)
_cell_length_c                   12.8929(12)
_cell_measurement_reflns_used    49270
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      2.437
_cell_volume                     5342.7(12)
_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_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_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     0.7108
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_av_unetI/netI     0.1753
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            49270
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.437
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       plate
_exptl_crystal_F_000             2078
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
In order to subtract the contribution from the disordered 
solvent (ethanol), the SQUEEZE command was applied, 
which gave a new HKL file. The number of located electrons is 
554 which equates to approximately 12 ethanol molecules 
per unit cell and 3 per asymmetric unit. This has been
added to the reported formula (as have the hydrogen atoms
not located on the coordinated water).
;
_refine_diff_density_max         0.900
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         12282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.0770
_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^)+(0.0986P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1878
_refine_ls_wR_factor_ref         0.2169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6020
_reflns_number_total             12282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02896_si_001.cif
_cod_data_source_block           MnMOF[Mn(CO)3(H2O)]Br
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5342.6(11)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C45 H52 Br0.50 Mn2 N6 O11'
_cod_database_code               4132310
_shelx_estimated_absorpt_t_min   0.714
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2014/6
_shelx_res_checksum              25411
_shelx_hkl_checksum              23167