Cubane and dicubane complexes stabilised by sterically demanding m-terphenyl ligands
Benjamin M. Gridley; Toby J. Blundell; Graeme J. Moxey; William Lewis; Alexander J. Blake; Deborah L. Kays; Chem.Commun. 49 (2013) 9752–; doi:10.1039/c3cc46384b

data_7109909
_publ_section_title
;
 Cubane and dicubane complexes stabilised by sterically demanding
 m-terphenyl ligands
;
_journal_name_full               Chem.Commun.
_journal_page_first              9752
_journal_paper_doi               10.1039/c3cc46384b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C104 H116 Cd5 Cl8 Li2 O2, 2(C4 H8 O)'
_chemical_formula_sum            'C112 H132 Cd5 Cl8 Li2 O4'
_chemical_formula_weight         2401.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL-97 created file'
_cell_angle_alpha                90.00
_cell_angle_beta                 103.9790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.3276(11)
_cell_length_b                   20.5180(15)
_cell_length_c                   17.4669(12)
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.32
_cell_volume                     5678.3(7)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    ' ? '
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27903
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2436
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
A disordered uncoordinated THF molecule was identified in the difference map, 
but a sensible disorder model could not be developed, so this was removed using 
PLATON SQUEEZE.
;
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         9993
_refine_ls_number_restraints     1728
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0928
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+21.9189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1978
_refine_ls_wR_factor_ref         0.2104
_reflns_number_gt                7502
_reflns_number_total             9993
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3cc46384b.txt
_cod_data_source_block           3.2THF
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7109909
_nottingham_internal_coll_name   CDBG2A
_nottingham_internal_coll_number 9032
_nottingham_internal_coll_client BG2/DLK
_nottingham_internal_coll_type   hemisphere
_nottingham_internal_coll_frame_time '60 s'
_nottingham_internal_coll_frame_width '0.3 degrees'
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   BG
_nottingham_internal_coll_date   10/6/2010
_nottingham_internal_process_user BG
_nottingham_internal_process_date 11/06/2010
_nottingham_internal_solution_user bmg
_nottingham_internal_solution_date 1/6/2010
_nottingham_internal_refinement_user wl/bmg
_nottingham_internal_refinement_date 22/11/2010
_nottingham_internal_validation_user wl
_nottingham_internal_validation_date 22/11/2010
_nottingham_internal_archive_date 23/11/2010