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_4132307
_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            'C27 H30 Mn N7 O7'
_chemical_formula_weight         619.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                76.778(7)
_cell_angle_beta                 74.207(7)
_cell_angle_gamma                84.676(6)
_cell_formula_units_Z            2
_cell_length_a                   9.2015(7)
_cell_length_b                   10.7157(8)
_cell_length_c                   15.6589(12)
_cell_measurement_reflns_used    2901
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0930
_cell_measurement_theta_min      3.8430
_cell_volume                     1445.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -54.00  45.00   1.00   50.00    --   18.87 -37.00 -90.00   99
  2  \w     -7.00  91.00   1.00   50.00    --   18.87  37.00  90.00   98
  3  \w     32.00  95.00   1.00   50.00    --   18.87-178.00 -30.00   63
  4  \w    -25.00  22.00   1.00   50.00    --  -19.50 -99.00  60.00   47
  5  \w    -88.00   2.00   1.00   50.00    --  -19.50 -57.00 120.00   90
  6  \w    -25.00  22.00   1.00   50.00    --  -19.50 -99.00-120.00   47
  7  \w    -25.00  55.00   1.00   50.00    --   18.87 -99.00 120.00   80
  8  \w    -50.00 -25.00   1.00   50.00    --   18.87 -57.00 150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24604
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.290
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       rod
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0336P)^2^+0.4151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4675
_reflns_number_total             6289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02896_si_001.cif
_cod_data_source_block           '[MnL(CO)3(DMT)]'
_cod_database_code               4132307
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.975
_shelxl_version_number           2014/6
_shelx_res_checksum              83630
_shelx_hkl_checksum              80742