Inflating face-capped Pd<sub>6</sub>L<sub>8</sub> coordination cages.
Jansze, Suzanne M.; Ortiz, Daniel; Fadaei Tirani, Farzaneh; Scopelliti, Rosario; Menin, Laure; Severin, Kay; Chemical communications (Cambridge, England) 54 (2018) 9529–9532; doi:10.1039/c8cc04870c

data_7122146
_publ_section_title
;
 Inflating face-capped Pd<sub>6</sub>L<sub>8</sub> coordination cages.
;
_journal_issue                   68
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9529
_journal_page_last               9532
_journal_paper_doi               10.1039/c8cc04870c
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C75 H87 B6 Fe3 N21 O18'
_chemical_formula_sum            'C75 H87 B6 Fe3 N21 O18'
_chemical_formula_weight         1803.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-06-15 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.551(3)
_cell_length_b                   9.2730(6)
_cell_length_c                   29.6345(18)
_cell_measurement_reflns_used    6517
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.6320
_cell_measurement_theta_min      4.7390
_cell_volume                     9769.4(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -110.00 -14.00   1.00   10.00    --  -42.01 -57.00  90.00   96
  2  \w   -115.00 -30.00   1.00   10.00    --  -42.01 -37.00-120.00   85
  3  \w   -116.00 -18.00   1.00   10.00    --  -42.01 -37.00 -30.00   98
  4  \w    -63.00  -2.00   1.00   10.00    --  -42.01  57.00-120.00   61
  5  \w      9.00  37.00   1.00   10.00    --   42.01  77.00  90.00   28
  6  \w     35.00  98.00   1.00   10.00    --   42.01-125.00 -30.00   63
  7  \w    106.00 169.00   1.00   40.00    --  110.51 125.00-120.00   63
  8  \w     51.00 119.00   1.00   40.00    --  110.51-125.00 -60.00   68
  9  \w     45.00 132.00   1.00   40.00    --  110.51 -61.00 -90.00   87
 10  \w     28.00  54.00   1.00   40.00    --  110.51 -94.00 -60.00   26
 11  \w     77.00 108.00   1.00   40.00    --  110.51 -94.00 -60.00   31
 12  \w    101.00 148.00   1.00   40.00    --  110.51 126.00 -84.00   47
 13  \w     92.00 177.00   1.00   40.00    --  110.51  45.00   0.00   85
 14  \w     41.00  66.00   1.00   40.00    --  110.51 -45.00 120.00   25
 15  \w     40.00  99.00   1.00   40.00    --  110.51-125.00-120.00   59
 16  \w     67.00  96.00   1.00   40.00    --  110.51 -94.00  30.00   29
 17  \w     90.00 115.00   1.00   40.00    --  110.51 -45.00 120.00   25
 18  \w     46.00 121.00   1.00   40.00    --  110.51 -30.00 -30.00   75
 19  \w     64.00 122.00   1.00   40.00    --  110.51-125.00 120.00   58
 20  \w     31.00 162.00   1.00   40.00    --  110.51 -15.00-180.00  131
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1146
_diffrn_reflns_av_unetI/netI     0.0888
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            62177
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        65.086
_diffrn_reflns_theta_max         65.086
_diffrn_reflns_theta_min         3.884
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.101
_exptl_absorpt_correction_T_max  0.715
_exptl_absorpt_correction_T_min  0.128
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       prism
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.610
_exptl_crystal_size_mid          0.448
_exptl_crystal_size_min          0.192
_refine_diff_density_max         2.009
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.484(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         16099
_refine_ls_number_restraints     3070
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.1235
_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^)+(0.1529P)^2^+78.9497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3170
_refine_ls_wR_factor_ref         0.3566
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.936
_reflns_number_gt                10367
_reflns_number_total             16099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04870c2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7122145--7122147.cif.'
_cod_original_cell_volume        9769.5(12)
_cod_database_code               7122146
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              12815
_shelx_fab_checksum              89100