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_7109908
_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         'C76 H83 Cd3 Cl3.68 I0.32 Li O, 0.25(C6 H14)'
_chemical_formula_sum            'C77.5 H86.5 Cd3 Cl3.68 I0.32 Li O'
_chemical_formula_weight         1548.74
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-16
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                84.2460(10)
_cell_angle_beta                 80.7940(10)
_cell_angle_gamma                62.9260(10)
_cell_formula_units_Z            4
_cell_length_a                   13.8697(7)
_cell_length_b                   14.0269(7)
_cell_length_c                   42.588(2)
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.22
_cell_volume                     7278.9(6)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            54094
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.869
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3143
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.755
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1853
_refine_ls_number_reflns         25643
_refine_ls_number_restraints     2249
_refine_ls_restrained_S_all      1.263
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0100P)^2^+43.9197P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23386
_reflns_number_total             25643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc46384b.txt
_cod_data_source_block           2.0.25C6H14
_cod_original_cell_volume        7279.0(7)
_cod_original_formula_sum        'C77.50 H86.50 Cd3 Cl3.68 I0.32 Li O'
_cod_database_code               7109908
_nottingham_internal_coll_name   CDBG2G
_nottingham_internal_coll_number 9915
_nottingham_internal_coll_client BG2/DLK
_nottingham_internal_coll_date   10/6/2010
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_frame_time '60 s'
_nottingham_internal_coll_frame_width '0.3 degrees'
_nottingham_internal_coll_type   hemisphere
_nottingham_internal_coll_user   BMG
_nottingham_internal_process_date 11/06/2010
_nottingham_internal_process_user BMG
_nottingham_internal_refinement_date 15/04/2013
_nottingham_internal_refinement_user BMG
_nottingham_internal_validation_date 16/05/2013
_nottingham_internal_validation_user WL
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cd1-Cl4 = Cd2-Cl4 = Cd3-Cl4
 2.7 with sigma of 0.01
 Cd1-I4 = Cd2-I4 = Cd3-I4
 2.98 with sigma of 0.01
 Cd4-Cl8 = Cd5-Cl8 = Cd6-Cl8
 2.7 with sigma of 0.01
 Cd4-I8 = Cd5-I8 = Cd6-I8
 2.98 with sigma of 0.01
 C170-O2 \\sim O2-C167
 with sigma of 0.02
 C76-O1 \\sim O1-C73
 with sigma of 0.02
 C75A-C76 \\sim C76-C75
 with sigma of 0.02
 C74-C73 \\sim C73-C74A
 with sigma of 0.02
 C75-C74 \\sim C74A-C75A
 with sigma of 0.02
 C74-O1 \\sim O1-C74A
 with sigma of 0.02
 C75-C73 \\sim C73-C75A
 with sigma of 0.02
 C74-C76 \\sim C74A-C76
 with sigma of 0.02
 C75A-O1 \\sim O1-C75
 with sigma of 0.02
 C172-C170 \\sim C170-C169
 with sigma of 0.02
 C171-C167 \\sim C167-C168
 with sigma of 0.02
 C172-C171 \\sim C169-C168
 with sigma of 0.02
 C169-O2 \\sim O2-C172
 with sigma of 0.02
 O2-C171 \\sim O2-C168
 with sigma of 0.02
 C170-C171 \\sim C170-C168
 with sigma of 0.02
 C167-C169 \\sim C167-C172
 with sigma of 0.02
 C201-C206 \\sim C201-C203 \\sim C206-C203 \\sim C202-C204 \\sim C203-C205
 with sigma of 0.02
 C206-C202 \\sim C202-C201 \\sim C203-C202 \\sim C204-C203 \\sim C205-C204
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and 
sigma for terminal atoms of 0.01
5. Others
 Sof(C75A)=Sof(H75C)=Sof(H75D)=Sof(H76C)=Sof(H76D)=1-FVAR(1)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H76A)=Sof(H76B)=FVAR(1)
 Sof(H16L)=Sof(H16M)=Sof(H17C)=Sof(H17D)=Sof(C171)=Sof(H17E)=Sof(H17F)=
 Sof(C172)=Sof(H17G)=Sof(H17H)=1-FVAR(2)
 Sof(H16J)=Sof(H16K)=Sof(C168)=Sof(H16N)=Sof(H16O)=Sof(C169)=Sof(H16P)=
 Sof(H16Q)=Sof(H17A)=Sof(H17B)=FVAR(2)
 Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74C)=Sof(H74D)=1-FVAR(3)
 Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=FVAR(3)
 Sof(C134)=Sof(C135)=Sof(C136)=Sof(H136)=Sof(C137)=Sof(C138)=Sof(H138)=
 Sof(C139)=Sof(C140)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C141)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=Sof(C142)=Sof(H14G)=Sof(H14H)=Sof(H14I)=1-FVAR(4)
 Sof(C125)=Sof(C126)=Sof(C127)=Sof(H127)=Sof(C128)=Sof(C129)=Sof(H129)=
 Sof(C130)=Sof(C131)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C132)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C133)=Sof(H13G)=Sof(H13H)=Sof(H13I)=FVAR(4)
 Sof(C101)=Sof(C102)=Sof(C103)=Sof(H103)=Sof(C104)=Sof(C105)=Sof(H105)=
 Sof(C106)=Sof(C107)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C108)=Sof(H10G)=
 Sof(H10H)=Sof(H10I)=Sof(C109)=Sof(H10J)=Sof(H10K)=Sof(H10L)=1-FVAR(5)
 Sof(C92)=Sof(C93)=Sof(C94)=Sof(H94)=Sof(C95)=Sof(C96)=Sof(H96)=Sof(C97)=
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=
 Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(5)
 Sof(I4)=1-FVAR(6)
 Sof(Cl4)=FVAR(6)
 Sof(I8)=1-FVAR(7)
 Sof(Cl8)=FVAR(7)
 Fixed Sof: C203(0.5) H20A(0.5) H20B(0.5) C204(0.5) H20C(0.5) H20D(0.5)
 C205(0.5) H20E(0.5) H20F(0.5) H20G(0.5) C202(0.5) H202(0.5) C201(0.5)
 H20H(0.5) H20I(0.5) H20J(0.5) C206(0.5) H20K(0.5) H20L(0.5) H20M(0.5)
6.a Ternary CH refined with riding coordinates:
 C202(H202)
6.b Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C73(H73C,H73D), C74(H74A,H74B), C74A(H74C,H74D), C75(H75A,
 H75B), C75A(H75C,H75D), C76(H76A,H76B), C76(H76C,H76D), C167(H16J,H16K),
 C167(H16L,H16M), C168(H16N,H16O), C169(H16P,H16Q), C170(H17A,H17B), C170(H17C,
 H17D), C171(H17E,H17F), C172(H17G,H17H), C203(H20A,H20B), C204(H20C,H20D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C18(H18), C20(H20), C27(H27),
 C28(H28), C29(H29), C33(H33), C35(H35), C42(H42), C44(H44), C51(H51), C52(H52),
  C53(H53), C57(H57), C59(H59), C66(H66), C68(H68), C79(H79), C80(H80),
 C81(H81), C85(H85), C87(H87), C94(H94), C96(H96), C103(H103), C105(H105),
 C112(H112), C113(H113), C114(H114), C118(H118), C120(H120), C127(H127),
 C129(H129), C136(H136), C138(H138), C145(H145), C146(H146), C147(H147),
 C151(H151), C153(H153), C160(H160), C162(H162)
6.d Idealised Me refined as rotating group:
 C13(H13J,H13K,H13L), C14(H14J,H14K,H14L), C15(H15J,H15K,H15L), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C89(H89A,
 H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C98(H98A,H98B,H98C),
 C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C107(H10D,H10E,H10F), C108(H10G,
 H10H,H10I), C109(H10J,H10K,H10L), C122(H12A,H12B,H12C), C123(H12D,H12E,H12F),
 C124(H12G,H12H,H12I), C131(H13A,H13B,H13C), C132(H13D,H13E,H13F), C133(H13G,
 H13H,H13I), C140(H14A,H14B,H14C), C141(H14D,H14E,H14F), C142(H14G,H14H,H14I),
 C155(H15A,H15B,H15C), C156(H15D,H15E,H15F), C157(H15G,H15H,H15I), C164(H16A,
 H16B,H16C), C165(H16D,H16E,H16F), C166(H16G,H16H,H16I), C205(H20E,H20F,H20G),
 C201(H20H,H20I,H20J), C206(H20K,H20L,H20M)
;
_shelxl_version_number           2013-2