#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:18:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178844 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/98/4109860.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4109860
loop_
_publ_author_name
'Zhongliang Zhu'
'Marcin Brynda'
'Robert J. Wright'
'Roland C. Fischer'
'W. Alexander Merrill'
'Eric Rivard'
'Robert Wolf'
'James C. Fettinger'
'Marilyn M. Olmstead'
'Philip P. Power'
_publ_contact_author_address
;
Department of Chemistry
University of California
Davis
CA 95616
UNITED STATES OF AMERICA
;
_publ_contact_author_email       PPPOWER@UCDAVIS.EDU
_publ_contact_author_name        'P. P. Power'
_publ_section_title
;
 Synthesis and Characterization of the Homologous M-M Bonded Series
 Ar'MMAr' (M = Zn, Cd, or Hg; Ar' = C6H3-2,6-(C6H3-2,6-Pri2)2) and Related
 Arylmetal Halides and Hydride Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10847
_journal_page_last               10857
_journal_paper_doi               10.1021/ja072682x
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C60 H76 Cd2'
_chemical_formula_sum            'C60 H76 Cd2'
_chemical_formula_weight         1022.01
_chemical_name_common            'Compound 9'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.5438(8)
_cell_length_b                   15.7065(6)
_cell_length_c                   16.3757(6)
_cell_measurement_reflns_used    7843
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.8088
_cell_measurement_theta_min      2.4875
_cell_volume                     5284.0(3)
_computing_cell_refinement       'SAINT (7.06a) (Bruker, 2004)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT (7.06a) (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            68282
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.8704
_exptl_absorpt_correction_T_min  0.8049
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2.10'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         4.470
_refine_diff_density_min         -1.958
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         7708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0487
_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/[σ²(Fo²)+(0.0572P)²+21.1464P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1437
_reflns_number_gt                5519
_reflns_number_total             7708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja072682xsi20070417_053248_6.cif
_cod_data_source_block           dippcdh
_cod_database_code               4109860
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cd1 Cd 0.454832(12) 0.505127(15) 0.068643(15) 0.02155(9) Uani 1 1 d .
H1 H 0.499(3) 0.415(4) 0.031(4) 0.066(18) Uiso 1 1 d .
C1 C 0.40891(15) 0.59379(18) 0.14703(18) 0.0148(5) Uani 1 1 d .
C2 C 0.34534(14) 0.58401(18) 0.17646(18) 0.0147(5) Uani 1 1 d .
C3 C 0.32027(15) 0.6405(2) 0.23456(19) 0.0178(6) Uani 1 1 d .
H3 H 0.2769 0.6340 0.2538 0.021 Uiso 1 1 calc R
C4 C 0.35909(16) 0.7063(2) 0.2641(2) 0.0199(6) Uani 1 1 d .
H4 H 0.3422 0.7444 0.3038 0.024 Uiso 1 1 calc R
C5 C 0.42254(15) 0.71661(19) 0.23588(19) 0.0175(6) Uani 1 1 d .
H5 H 0.4488 0.7616 0.2564 0.021 Uiso 1 1 calc R
C6 C 0.44755(14) 0.66078(18) 0.17737(18) 0.0138(5) Uani 1 1 d .
C7 C 0.51532(14) 0.66888(18) 0.14443(18) 0.0154(5) Uani 1 1 d .
C8 C 0.52912(16) 0.72867(19) 0.08267(19) 0.0179(6) Uani 1 1 d .
C9 C 0.59100(17) 0.7288(2) 0.0468(2) 0.0254(7) Uani 1 1 d .
H9 H 0.6005 0.7686 0.0048 0.030 Uiso 1 1 calc R
C10 C 0.63805(18) 0.6723(2) 0.0712(3) 0.0311(8) Uani 1 1 d .
H10 H 0.6797 0.6732 0.0461 0.037 Uiso 1 1 calc R
C11 C 0.62502(17) 0.6140(2) 0.1326(3) 0.0286(8) Uani 1 1 d .
H11 H 0.6580 0.5754 0.1494 0.034 Uiso 1 1 calc R
C12 C 0.56405(16) 0.6110(2) 0.1700(2) 0.0204(6) Uani 1 1 d .
C19 C 0.30485(14) 0.51161(19) 0.14405(18) 0.0155(5) Uani 1 1 d .
C20 C 0.26251(15) 0.5256(2) 0.07750(19) 0.0174(6) Uani 1 1 d .
C21 C 0.22659(17) 0.4568(2) 0.0468(2) 0.0242(7) Uani 1 1 d .
H21 H 0.1978 0.4654 0.0022 0.029 Uiso 1 1 calc R
C22 C 0.23264(18) 0.3763(2) 0.0808(2) 0.0272(7) Uani 1 1 d .
H22 H 0.2076 0.3303 0.0600 0.033 Uiso 1 1 calc R
C23 C 0.27507(17) 0.3631(2) 0.1450(2) 0.0261(7) Uani 1 1 d .
H23 H 0.2793 0.3076 0.1675 0.031 Uiso 1 1 calc R
C24 C 0.31172(16) 0.4295(2) 0.1774(2) 0.0197(6) Uani 1 1 d .
C16 C 0.47789(17) 0.7906(2) 0.0507(2) 0.0212(6) Uani 1 1 d .
H16 H 0.4396 0.7880 0.0883 0.025 Uiso 1 1 calc R
C17 C 0.4547(2) 0.7639(3) -0.0342(2) 0.0339(8) Uani 1 1 d .
H17A H 0.4921 0.7603 -0.0712 0.051 Uiso 1 1 calc R
H17B H 0.4237 0.8060 -0.0550 0.051 Uiso 1 1 calc R
H17C H 0.4335 0.7081 -0.0308 0.051 Uiso 1 1 calc R
C18 C 0.5026(2) 0.8827(2) 0.0497(2) 0.0299(8) Uani 1 1 d .
H18A H 0.5166 0.8989 0.1048 0.045 Uiso 1 1 calc R
H18B H 0.4675 0.9207 0.0319 0.045 Uiso 1 1 calc R
H18C H 0.5394 0.8875 0.0120 0.045 Uiso 1 1 calc R
C13 C 0.55254(17) 0.5498(2) 0.2409(2) 0.0227(6) Uani 1 1 d .
H13 H 0.5048 0.5378 0.2436 0.027 Uiso 1 1 calc R
C14 C 0.5719(3) 0.5927(3) 0.3203(3) 0.0434(11) Uani 1 1 d .
H14A H 0.5637 0.5539 0.3660 0.065 Uiso 1 1 calc R
H14B H 0.5463 0.6447 0.3276 0.065 Uiso 1 1 calc R
H14C H 0.6183 0.6072 0.3186 0.065 Uiso 1 1 calc R
C15 C 0.5876(3) 0.4646(3) 0.2321(3) 0.0442(11) Uani 1 1 d .
H15A H 0.6346 0.4735 0.2368 0.066 Uiso 1 1 calc R
H15B H 0.5776 0.4399 0.1785 0.066 Uiso 1 1 calc R
H15C H 0.5730 0.4258 0.2751 0.066 Uiso 1 1 calc R
C25 C 0.35704(17) 0.4116(2) 0.2488(2) 0.0217(6) Uani 1 1 d .
H25 H 0.3845 0.4633 0.2579 0.026 Uiso 1 1 calc R
C26 C 0.3176(2) 0.3953(3) 0.3266(2) 0.0355(9) Uani 1 1 d .
H26A H 0.2902 0.4450 0.3383 0.053 Uiso 1 1 calc R
H26B H 0.3473 0.3855 0.3724 0.053 Uiso 1 1 calc R
H26C H 0.2900 0.3451 0.3189 0.053 Uiso 1 1 calc R
C27 C 0.4023(2) 0.3366(3) 0.2318(2) 0.0343(9) Uani 1 1 d .
H27A H 0.3768 0.2840 0.2288 0.051 Uiso 1 1 calc R
H27B H 0.4344 0.3318 0.2759 0.051 Uiso 1 1 calc R
H27C H 0.4249 0.3457 0.1798 0.051 Uiso 1 1 calc R
C28 C 0.25560(18) 0.6127(2) 0.0387(2) 0.0228(6) Uani 1 1 d .
H28 H 0.2897 0.6501 0.0634 0.027 Uiso 1 1 calc R
C30 C 0.1900(3) 0.6509(3) 0.0603(5) 0.0658(19) Uani 1 1 d .
H30A H 0.1872 0.7088 0.0381 0.099 Uiso 1 1 calc R
H30B H 0.1852 0.6529 0.1198 0.099 Uiso 1 1 calc R
H30C H 0.1553 0.6158 0.0369 0.099 Uiso 1 1 calc R
C29 C 0.2673(4) 0.6113(3) -0.0525(3) 0.067(2) Uani 1 1 d .
H29A H 0.3104 0.5872 -0.0636 0.101 Uiso 1 1 calc R
H29B H 0.2651 0.6694 -0.0739 0.101 Uiso 1 1 calc R
H29C H 0.2339 0.5762 -0.0789 0.101 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Cd1 Cd1 141.89(8) . 5_665
C1 Cd1 H1 163(2) . .
Cd1 Cd1 H1 50.9(19) 5_665 .
C2 C1 C6 119.1(3) . .
C2 C1 Cd1 123.5(2) . .
C6 C1 Cd1 117.0(2) . .
C3 C2 C1 120.5(3) . .
C3 C2 C19 121.0(3) . .
C1 C2 C19 118.5(3) . .
C4 C3 C2 119.7(3) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C3 C4 C5 120.5(3) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
C4 C5 C6 119.9(3) . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C5 C6 C1 120.2(3) . .
C5 C6 C7 122.4(3) . .
C1 C6 C7 117.4(3) . .
C8 C7 C12 119.9(3) . .
C8 C7 C6 120.1(3) . .
C12 C7 C6 119.8(3) . .
C9 C8 C7 119.0(3) . .
C9 C8 C16 118.8(3) . .
C7 C8 C16 122.2(3) . .
C10 C9 C8 121.1(3) . .
C10 C9 H9 119.5 . .
C8 C9 H9 119.5 . .
C9 C10 C11 120.2(3) . .
C9 C10 H10 119.9 . .
C11 C10 H10 119.9 . .
C10 C11 C12 120.9(3) . .
C10 C11 H11 119.6 . .
C12 C11 H11 119.6 . .
C11 C12 C7 119.0(3) . .
C11 C12 C13 119.6(3) . .
C7 C12 C13 121.3(3) . .
C24 C19 C20 120.3(3) . .
C24 C19 C2 120.0(3) . .
C20 C19 C2 119.7(3) . .
C21 C20 C19 118.7(3) . .
C21 C20 C28 119.8(3) . .
C19 C20 C28 121.5(3) . .
C22 C21 C20 120.8(3) . .
C22 C21 H21 119.6 . .
C20 C21 H21 119.6 . .
C23 C22 C21 119.9(3) . .
C23 C22 H22 120.1 . .
C21 C22 H22 120.1 . .
C22 C23 C24 121.3(3) . .
C22 C23 H23 119.3 . .
C24 C23 H23 119.3 . .
C23 C24 C19 119.0(3) . .
C23 C24 C25 119.0(3) . .
C19 C24 C25 122.0(3) . .
C8 C16 C17 110.6(3) . .
C8 C16 C18 112.1(3) . .
C17 C16 C18 110.7(3) . .
C8 C16 H16 107.7 . .
C17 C16 H16 107.7 . .
C18 C16 H16 107.7 . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C14 C13 C15 110.3(3) . .
C14 C13 C12 109.3(3) . .
C15 C13 C12 114.0(3) . .
C14 C13 H13 107.7 . .
C15 C13 H13 107.7 . .
C12 C13 H13 107.7 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C24 C25 C27 112.1(3) . .
C24 C25 C26 110.3(3) . .
C27 C25 C26 110.2(3) . .
C24 C25 H25 108.0 . .
C27 C25 H25 108.0 . .
C26 C25 H25 108.0 . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C25 C27 H27A 109.5 . .
C25 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C25 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C29 C28 C20 112.7(3) . .
C29 C28 C30 112.1(5) . .
C20 C28 C30 110.1(3) . .
C29 C28 H28 107.2 . .
C20 C28 H28 107.2 . .
C30 C28 H28 107.2 . .
C28 C30 H30A 109.5 . .
C28 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C28 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C28 C29 H29A 109.5 . .
C28 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C28 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 C1 2.116(3) .
Cd1 Cd1 2.9196(5) 5_665
Cd1 H1 1.79(6) .
C1 C2 1.401(4) .
C1 C6 1.409(4) .
C2 C3 1.399(4) .
C2 C19 1.506(4) .
C3 C4 1.392(4) .
C3 H3 0.9500 .
C4 C5 1.393(4) .
C4 H4 0.9500 .
C5 C6 1.397(4) .
C5 H5 0.9500 .
C6 C7 1.499(4) .
C7 C8 1.409(4) .
C7 C12 1.415(4) .
C8 C9 1.401(4) .
C8 C16 1.526(5) .
C9 C10 1.372(5) .
C9 H9 0.9500 .
C10 C11 1.386(5) .
C10 H10 0.9500 .
C11 C12 1.395(5) .
C11 H11 0.9500 .
C12 C13 1.527(5) .
C19 C24 1.407(4) .
C19 C20 1.412(4) .
C20 C21 1.403(5) .
C20 C28 1.514(4) .
C21 C22 1.387(5) .
C21 H21 0.9500 .
C22 C23 1.381(5) .
C22 H22 0.9500 .
C23 C24 1.392(5) .
C23 H23 0.9500 .
C24 C25 1.521(5) .
C16 C17 1.527(5) .
C16 C18 1.533(5) .
C16 H16 1.0000 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C13 C14 1.518(5) .
C13 C15 1.526(5) .
C13 H13 1.0000 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C25 C27 1.527(5) .
C25 C26 1.531(5) .
C25 H25 1.0000 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 C29 1.513(6) .
C28 C30 1.516(6) .
C28 H28 1.0000 .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
