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_7124993
_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         'C44 H40 B2 Fe N10 O6'
_chemical_formula_sum            'C44 H40 B2 Fe N10 O6'
_chemical_formula_weight         882.33
_chemical_name_systematic        gc2_203
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2016-07-22 deposited with the CCDC.
2016-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.425(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4866(4)
_cell_length_b                   10.6979(3)
_cell_length_c                   47.959(2)
_cell_measurement_reflns_used    11289
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      74.7100
_cell_measurement_theta_min      4.5090
_cell_volume                     4852.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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   -109.00 -16.00   1.00    5.50    --  -40.79 -38.00  30.00   93
  2  \w    -57.00  33.00   1.00    5.50    --  -40.79  38.00 -60.00   90
  3  \w   -115.00 -19.00   1.00    5.50    --  -40.79 -38.00 -60.00   96
  4  \w     24.00  90.00   1.00    5.50    --   40.79-125.00-150.00   66
  5  \w     48.00  95.00   1.00    5.50    --   40.79-125.00  30.00   47
  6  \w    -29.00  62.00   1.00    5.50    --   40.79 -38.00 120.00   91
  7  \w     37.00 130.00   1.00   22.00    --  110.60 -30.00-150.00   93
  8  \w     80.00 128.00   1.00   22.00    --  110.60 -61.00 -30.00   48
  9  \w     42.00 143.00   1.00   22.00    --  110.60 -77.00 150.00  101
 10  \w     29.00  56.00   1.00   22.00    --  110.60 -94.00-150.00   27
 11  \w     85.00 177.00   1.00   22.00    --  110.60  45.00-120.00   92
 12  \w     31.00  65.00   1.00   22.00    --  110.60 -94.00 150.00   34
 13  \w     87.00 118.00   1.00   22.00    --  110.60-125.00 -60.00   31
 14  \w     39.00 118.00   1.00   22.00    --  110.60 -30.00 -60.00   79
 15  \w     47.00 122.00   1.00   22.00    --  110.60-125.00 150.00   75
 16  \w     37.00  98.00   1.00   22.00    --  110.60 -94.00 -30.00   61
 17  \w     54.00 104.00   1.00   22.00    --  110.60 -94.00   0.00   50
 18  \w     31.00 141.00   1.00   22.00    --  110.60 -15.00  60.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_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  0.0614
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            34528
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.611
_diffrn_reflns_theta_min         3.698
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.936
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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 pale orange'
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0807
_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^)+(0.0348P)^2^+19.5319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1791
_refine_ls_wR_factor_ref         0.1824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8963
_reflns_number_total             9908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06066h2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7124993
_shelx_shelxl_version_number     2016/4
_shelx_res_checksum              33706
_shelx_hkl_checksum              74603
_shelx_fab_checksum              45009