Large heterometallic coordination cages with gyrobifastigium-like geometry.
Cecot, Giacomo; Alameddine, Bassam; Prior, Stéphanie; Zorzi, Rita De; Geremia, Silvano; Scopelliti, Rosario; Fadaei, Farzaneh T.; Solari, Euro; Severin, Kay; Chemical communications (Cambridge, England) 52 (2016) 11243–11246; doi:10.1039/c6cc06066h

data_7124991
_publ_section_title
;
 Large heterometallic coordination cages with gyrobifastigium-like
 geometry.
;
_journal_issue                   75
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11243
_journal_page_last               11246
_journal_paper_doi               10.1039/c6cc06066h
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'C392 H368 B8 Fe4 N40 O24 P16 Pt8, 16(C F3 O3 S)'
_chemical_formula_sum            'C408 H368 B8 F48 Fe4 N40 O72 P16 Pt8 S16'
_chemical_formula_weight         10774.48
_chemical_name_systematic        gc2_222
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-16
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-13 deposited with the CCDC.
2016-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                101.861(4)
_cell_angle_beta                 92.914(4)
_cell_angle_gamma                104.120(4)
_cell_formula_units_Z            2
_cell_length_a                   28.3614(16)
_cell_length_b                   28.8276(11)
_cell_length_c                   41.0379(16)
_cell_measurement_reflns_used    15502
_cell_measurement_temperature    139.99(14)
_cell_measurement_theta_max      50.2320
_cell_measurement_theta_min      3.5050
_cell_volume                     31663(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      139.99(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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    -24.00  30.00   1.00   12.50    --    0.00 -77.00 120.00   54
  2  \w    -15.00  85.00   1.00   50.00    --   60.31 -77.00  30.00  100
  3  \w     26.00  80.00   1.00   50.00    --   60.31 -77.00 -30.00   54
  4  \w     23.00 115.00   1.00   50.00    --   60.31-125.00 -60.00   92
  5  \w     57.00  89.00   1.00   50.00    --   60.31-125.00-180.00   32
  6  \w    -16.00  66.00   1.00   50.00    --   60.31 -77.00 -60.00   82
  7  \w    -12.00  81.00   1.00   50.00    --   60.31 -37.00  60.00   93
  8  \w     89.00 131.00   1.00   50.00    --   60.31  37.00 -30.00   42
  9  \w     96.00 121.00   1.00   50.00    --   60.31  37.00 -60.00   25
 10  \w     31.00 132.00   1.00   50.00    --   60.31  77.00-150.00  101
 11  \w      4.00  69.00   1.00   12.50    --    0.00  37.00 -30.00   65
 12  \w    -21.00  69.00   1.00   12.50    --    0.00  37.00 -90.00   90
 13  \w     -9.00  39.00   1.00   50.00    --   60.31 -37.00 150.00   48
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0329998000
_diffrn_orient_matrix_UB_12      0.0004298000
_diffrn_orient_matrix_UB_13      0.0286833000
_diffrn_orient_matrix_UB_21      0.0377401000
_diffrn_orient_matrix_UB_22      -0.0148037000
_diffrn_orient_matrix_UB_23      0.0213051000
_diffrn_orient_matrix_UB_31      0.0256878000
_diffrn_orient_matrix_UB_32      0.0545822000
_diffrn_orient_matrix_UB_33      0.0145472000
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.1853
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            67589
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        51.608
_diffrn_reflns_theta_max         51.608
_diffrn_reflns_theta_min         3.351
_exptl_absorpt_coefficient_mu    5.374
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             10736
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.358
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.155
_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     2775
_refine_ls_number_reflns         67589
_refine_ls_number_restraints     9293
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.2662
_refine_ls_R_factor_gt           0.1667
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+1000.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3590
_refine_ls_wR_factor_ref         0.4339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26255
_reflns_number_total             67589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06066h2.cif
_cod_data_source_block           global
_cod_database_code               7124991
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C306 H276 B6 N30 O54 F36 P12 S12 Fe3 Pt6'
_oxdiff_exptl_absorpt_empirical_full_min 0.512
_oxdiff_exptl_absorpt_empirical_full_max 2.309
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 96.57
_reflns_odcompleteness_theta     51.67
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              91667
_shelx_hkl_checksum              15367
_shelx_fab_checksum              90269