Ligand Aspect Ratio as a Decisive Factor for the Self-Assembly of Coordination Cages.
Jansze, Suzanne M.; Cecot, Giacomo; Wise, Matthew D.; Zhurov, Konstantin O.; Ronson, Tanya K.; Castilla, Ana M.; Finelli, Alba; Pattison, Philip; Solari, Euro; Scopelliti, Rosario; Zelinskii, Genrikh E.; Vologzhanina, Anna V.; Voloshin, Yan Z.; Nitschke, Jonathan R.; Severin, Kay; Journal of the American Chemical Society 138 (2016) 2046–2054; doi:10.1021/jacs.5b13190

data_4124907
_publ_section_title
;
 Ligand Aspect Ratio as a Decisive Factor for the Self-Assembly of
 Coordination Cages.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2046
_journal_page_last               2054
_journal_paper_doi               10.1021/jacs.5b13190
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C252 H252 B12 Fe10 N60 O36, 8(F6 Sb), 6(C3 H6 O)'
_chemical_formula_sum            'C270 H288 B12 F48 Fe10 N60 O42 Sb8'
_chemical_formula_weight         7619.81
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   28.0944(9)
_cell_length_b                   28.0944(9)
_cell_length_c                   184.156(7)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      88.663
_cell_measurement_theta_min      6.289
_cell_volume                     125880(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2013)'
_diffrn_ambient_temperature      135(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       125
_diffrn_reflns_limit_l_min       -167
_diffrn_reflns_number            70629
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        44.479
_diffrn_reflns_theta_max         44.479
_diffrn_reflns_theta_min         3.758
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.360
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             45888
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.230(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2537
_refine_ls_number_reflns         18720
_refine_ls_number_restraints     4821
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.1044
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1624P)^2^+4786.7290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2693
_refine_ls_wR_factor_ref         0.2811
_reflns_Friedel_coverage         0.999
_reflns_friedel_fraction_full    0.996
_reflns_friedel_fraction_max     0.996
_reflns_number_gt                16042
_reflns_number_total             18720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b13190_si_008.cif
_cod_data_source_block           jn1404_sq_s
_cod_depositor_comments
'Adding full bibliography for 4124901--4124909.cif.'
_cod_original_cell_volume        125879(9)
_cod_database_code               4124907
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.368
_shelx_estimated_absorpt_t_max   0.627
_shelx_res_checksum              99381
_shelx_hkl_checksum              69153
_shelx_fab_checksum              16886