Self-assembly of tetrareduced corannulene with mixed Li‒Rb clusters: dynamic transformations, unique structures and record7Li NMR shifts
Filatov, Alexander S.; Spisak, Sarah N.; Zabula, Alexander V.; McNeely, James; Rogachev, Andrey Yu.; Petrukhina, Marina A.; Chem. Sci. 6 (2015) 1959–; doi:10.1039/C4SC03485F

data_1518448
_publ_section_title
;
 Self-assembly of tetrareduced corannulene with mixed Li--Rb clusters:
 dynamic transformations, unique structures and record7Li NMR shifts
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              1959
_journal_paper_doi               10.1039/C4SC03485F
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C60 H60 Li4 O5 Rb4'
_chemical_formula_sum            'C60 H60 Li4 O5 Rb4'
_chemical_formula_weight         1230.72
_chemical_name_systematic
; 
  bis(m6-h1:h5:h6:h6:h6:h6-Corannulene)-
-(tetrahydrofuran-O,O)-bis(tetrahydrofuran-O,O,O)-
-tetra-lithium-tetra-rubidium 

;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      63
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-31 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.166(7)
_cell_length_b                   13.519(7)
_cell_length_c                   25.901(13)
_cell_measurement_reflns_used    1506
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.28
_cell_measurement_theta_min      2.84
_cell_volume                     4960(4)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30\% \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1667
_diffrn_reflns_av_sigmaI/netI    0.1038
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17450
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    3.975
_exptl_absorpt_correction_T_max  0.8900
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.624
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2347
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+114.3836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2331
_reflns_number_gt                1372
_reflns_number_total             2347
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4sc03485f2.cif
_cod_data_source_block           Li4Rb2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 1518448--1518449.cif.
;
_cod_original_sg_symbol_Hall     '-C 2c 2     '
_cod_original_sg_symbol_H-M      'C m c m     '
_cod_database_code               1518448