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_4124901
_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         'C28 H38 B2 Fe N8 O6'
_chemical_formula_sum            'C28 H38 B2 Fe N8 O6'
_chemical_formula_weight         660.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.044(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.958(3)
_cell_length_b                   8.8720(13)
_cell_length_c                   16.619(2)
_cell_measurement_reflns_used    183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     3643.7(8)
_computing_cell_refinement
'Dirax/lsq (Duisenberg and Schreurs, 1988-2000)'
_computing_data_collection       'collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg and Schreurs, 1990-2000)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\p and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20342
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.200
_diffrn_reflns_theta_max         27.573
_diffrn_reflns_theta_min         2.439
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0855 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.6937.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.555
_exptl_crystal_size_mid          0.416
_exptl_crystal_size_min          0.375
_refine_diff_density_max         1.723
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0929
_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^)+(0.0398P)^2^+43.2301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2150
_refine_ls_wR_factor_ref         0.2207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3429
_reflns_number_total             4133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b13190_si_005.cif
_cod_data_source_block           gc1-3
_cod_depositor_comments
'Adding full bibliography for 4124901--4124909.cif.'
_cod_database_code               4124901
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(H16E)=1-FVAR(1)
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C16A)=Sof(H16A)=Sof(H16B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C16A(H16A,H16B), C13B(H13D,H13E)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C16B(H16C,
 H16D,H16E)
;
_shelx_res_checksum              35973
_shelx_hkl_checksum              81132
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20