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_7109907
_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_absolute_configuration ad
_chemical_formula_moiety         'C64 H82 Cd2 I4 Li2 O2, C4 H8 O'
_chemical_formula_sum            'C68 H90 Cd2 I4 Li2 O3'
_chemical_formula_weight         1701.67
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5363(4)
_cell_length_b                   12.5363(4)
_cell_length_c                   43.668(2)
_cell_measurement_reflns_used    21142
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.14
_cell_volume                     6862.8(4)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_unetI/netI     0.021
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            81717
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.20
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.461
_exptl_absorpt_correction_T_max  0.357
_exptl_absorpt_correction_T_min  0.288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/2 (Bruker,2007) was used for absorption correction.
wR2(int) was 0.1131 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.8071.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.95
_refine_diff_density_rms         0.09
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.14
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7621
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.16
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0162P)^2^+25.713P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6625
_reflns_number_total             7621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc46384b.txt
_cod_data_source_block           1.THF
_cod_original_cell_volume        6862.9(5)
_cod_database_code               7109907
_nottingham_internal_coll_name   CDTBLC
_nottingham_internal_coll_number 11233
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_time 15
_nottingham_internal_coll_frame_width '0.3, 0.5'
_nottingham_internal_coll_frame_method '\w '
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   07/03/2012
_nottingham_internal_coll_location NOTT
_nottingham_internal_process_user TB
_nottingham_internal_process_date 07/03/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 29/05/2013
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 29/05/2013
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 31/05/2013
_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. Restrained distances
 O1-Li1 \\sim O2-Li1
 with sigma of 0.02
 O2-C32A \\sim O1-C32 \\sim O1-C29 \\sim O2-C29A
 with sigma of 0.02
 C30-C29 \\sim C29A-C30A \\sim C31A-C32A \\sim C31-C32
 with sigma of 0.02
 C31A-C30A \\sim C30-C31
 with sigma of 0.02
 O3-C33 \\sim O3-C33_$1 \\sim O3_$1-C33 \\sim O3_$1-C33_$1
 with sigma of 0.02
 O3-C36 \\sim O3-C33 \\sim O2-C29A \\sim O2-C32A \\sim O1-C29 \\sim O1-C32
 with sigma of 0.02
 C31A-C32A \\sim C31-C32 \\sim C29A-C30A \\sim C30-C29 \\sim C36-C35 
 \\sim C33-C34
 with sigma of 0.02
 C35-C34 \\sim C31A-C30A \\sim C30-C31
 with sigma of 0.02
3. Rigid bond restraints
 O2, C32A, C30A, C31A, C29A, O1, C32, C29, C31, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34, O3, C33, C36, C35
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
O2 \\sim C32A \\sim C30A \\sim C31A \\sim C29A \\sim O1 \\sim C32 \\sim C29 
\\sim C31 \\sim C30: within 1.7A with sigma of 0.04 and sigma for terminal 
atoms of 0.08
C34 \\sim O3 \\sim C33 \\sim C36 \\sim C35: within 1.7A with sigma of 0.01 
and sigma for terminal atoms of 0.02
5. Others
 Sof(O1)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=1-FVAR(1)
 Sof(O2)=Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=
 Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=FVAR(1)
 Fixed Sof: O3(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5)
 C35(0.5) H35A(0.5) H35B(0.5) C36(0.5) H36A(0.5) H36B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C29A(H29C,H29D), C30(H30A,H30B), C30A(H30C,H30D), C31(H31A,
 H31B), C31A(H31C,H31D), C32(H32A,H32B), C32A(H32C,H32D), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              6665
_shelxl_version_number           2013-2