X-ray Snapshot Observation of Palladium-Mediated Aromatic Bromination in a Porous Complex.
Ikemoto, Koki; Inokuma, Yasuhide; Rissanen, Kari; Fujita, Makoto; Journal of the American Chemical Society 136 (2014) 6892–6895; doi:10.1021/ja502996h

data_4121769
_publ_contact_author             'Makoto Fujita'
_publ_section_title
;
 X-ray Snapshot Observation of Palladium-Mediated Aromatic Bromination in
 a Porous Complex.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6892
_journal_page_last               6895
_journal_paper_doi               10.1021/ja502996h
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C60.19 H44.78 I6 N15.59 O Pd S2 Zn3'
_chemical_formula_weight         2130.50
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.774(3)
_cell_length_b                   13.8933(16)
_cell_length_c                   44.585(5)
_cell_measurement_reflns_used    7566
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.34
_cell_measurement_theta_min      2.45
_cell_volume                     17204(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            182442
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.272
_diffrn_reflns_theta_min         1.466
_exptl_absorpt_coefficient_mu    3.276
_exptl_absorpt_correction_T_max  0.8534
_exptl_absorpt_correction_T_min  0.6754
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8073
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6518
_platon_squeeze_details
;
;
_refine_diff_density_max         1.931
_refine_diff_density_min         -1.754
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         19203
_refine_ls_number_restraints     479
_refine_ls_restrained_S_all      0.870
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1059P)^2^+243.9696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2142
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12699
_reflns_number_total             19203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja502996h_si_003.cif
_cod_data_source_block           pbca
_cod_depositor_comments
;Adding full bibliography for 4121766--4121769.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4121769
_shelx_estimated_absorpt_t_min   0.675
_shelx_estimated_absorpt_t_max   0.853
_shelxl_version_number           2013-4
_shelx_res_checksum              80988
_shelx_hkl_checksum              57558