#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:51:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179158 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/19/4311997.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_4311997
loop_
_publ_author_name
'Shirley Hino'
'Marilyn Olmstead'
'Andrew D. Phillips'
'Robert J. Wright'
'Philip P. Power'
_publ_section_title
;
 Terphenyl Ligand Stabilized Lead(II) Derivatives: Steric Effects and
 Lead-Lead Bonding in Diplumbenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7346
_journal_page_last               7352
_journal_paper_doi               10.1021/ic049174y
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C60 H74 Br2 Pb2'
_chemical_formula_weight         1369.40
_chemical_name_common            (Ar'PbBr)2
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.539(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3164(18)
_cell_length_b                   14.1792(18)
_cell_length_c                   14.6144(18)
_cell_measurement_reflns_used    932
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.289
_cell_measurement_theta_min      2.4185
_cell_volume                     2735.6(6)
_computing_cell_refinement       'Bruker SAINT 6.33B (Bruker 2002)'
_computing_data_collection       'Bruker SMART 5.054 (Bruker 2001)'
_computing_data_reduction        'Bruker SAINT 6.33B (Bruker 2002)'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26755
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time
;
frames measured at beginning and end of data collection 
;
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    7.643
_exptl_absorpt_correction_T_max  0.4869
_exptl_absorpt_correction_T_min  0.4607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.04 (Sheldrick 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0274P)²+5.8623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                4780
_reflns_number_total             5340
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic049174ysi20040624_074118_1.cif
_cod_data_source_block           adp106
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4311997
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.608583(10) 0.606918(9) 0.013605(8) 0.01795(5) Uani 1 1 d . . .
Br1 Br 0.61219(3) 0.41601(2) 0.06616(2) 0.01814(8) Uani 1 1 d . . .
C1 C 0.6195(3) 0.6547(2) 0.1666(2) 0.0175(7) Uani 1 1 d . . .
C2 C 0.7159(3) 0.6933(2) 0.1938(2) 0.0204(7) Uani 1 1 d . . .
C3 C 0.7436(3) 0.7254(2) 0.2836(3) 0.0257(8) Uani 1 1 d . . .
H3A H 0.8084 0.7527 0.3011 0.031 Uiso 1 1 calc R . .
C4 C 0.6760(3) 0.7172(3) 0.3469(3) 0.0300(9) Uani 1 1 d . . .
H4A H 0.6949 0.7383 0.4085 0.036 Uiso 1 1 calc R . .
C5 C 0.5809(3) 0.6786(3) 0.3217(3) 0.0266(8) Uani 1 1 d . . .
H5A H 0.5357 0.6728 0.3665 0.032 Uiso 1 1 calc R . .
C6 C 0.5501(3) 0.6480(2) 0.2312(2) 0.0205(7) Uani 1 1 d . . .
C7 C 0.7895(3) 0.6990(2) 0.1233(2) 0.0213(7) Uani 1 1 d . . .
C8 C 0.8638(3) 0.6284(3) 0.1213(3) 0.0245(8) Uani 1 1 d . . .
C9 C 0.9278(3) 0.6316(3) 0.0527(3) 0.0341(9) Uani 1 1 d . . .
H9A H 0.9774 0.5838 0.0504 0.041 Uiso 1 1 calc R . .
C10 C 0.9200(4) 0.7028(3) -0.0114(3) 0.0428(11) Uani 1 1 d . . .
H10A H 0.9644 0.7042 -0.0573 0.051 Uiso 1 1 calc R . .
C11 C 0.8481(4) 0.7723(3) -0.0095(3) 0.0390(11) Uani 1 1 d . . .
H11A H 0.8434 0.8210 -0.0545 0.047 Uiso 1 1 calc R . .
C12 C 0.7820(3) 0.7728(3) 0.0569(3) 0.0287(9) Uani 1 1 d . . .
C13 C 0.8764(3) 0.5499(2) 0.1928(3) 0.0243(8) Uani 1 1 d . . .
H13A H 0.8105 0.5424 0.2180 0.029 Uiso 1 1 calc R . .
C14 C 0.9032(3) 0.4550(3) 0.1528(3) 0.0307(9) Uani 1 1 d . . .
H14A H 0.8513 0.4378 0.1017 0.046 Uiso 1 1 calc R . .
H14B H 0.9065 0.4066 0.2010 0.046 Uiso 1 1 calc R . .
H14C H 0.9691 0.4598 0.1302 0.046 Uiso 1 1 calc R . .
C15 C 0.9574(3) 0.5776(3) 0.2732(3) 0.0332(9) Uani 1 1 d . . .
H15A H 0.9396 0.6385 0.2985 0.050 Uiso 1 1 calc R . .
H15B H 1.0234 0.5827 0.2508 0.050 Uiso 1 1 calc R . .
H15C H 0.9607 0.5294 0.3216 0.050 Uiso 1 1 calc R . .
C16 C 0.7049(3) 0.8518(3) 0.0590(3) 0.0338(10) Uani 1 1 d . . .
H16A H 0.6494 0.8287 0.0932 0.041 Uiso 1 1 calc R . .
C17 C 0.6573(5) 0.8809(3) -0.0394(4) 0.0543(15) Uani 1 1 d . . .
H17A H 0.6265 0.8256 -0.0721 0.081 Uiso 1 1 calc R . .
H17B H 0.7101 0.9065 -0.0732 0.081 Uiso 1 1 calc R . .
H17C H 0.6053 0.9290 -0.0352 0.081 Uiso 1 1 calc R . .
C18 C 0.7528(3) 0.9383(3) 0.1093(3) 0.0374(10) Uani 1 1 d . . .
H18A H 0.7831 0.9202 0.1716 0.056 Uiso 1 1 calc R . .
H18B H 0.7007 0.9864 0.1134 0.056 Uiso 1 1 calc R . .
H18C H 0.8055 0.9638 0.0753 0.056 Uiso 1 1 calc R . .
C19 C 0.4418(3) 0.6198(3) 0.2022(2) 0.0235(8) Uani 1 1 d . . .
C20 C 0.4063(3) 0.5287(3) 0.2207(2) 0.0261(8) Uani 1 1 d . . .
C21 C 0.3058(3) 0.5068(3) 0.1893(3) 0.0326(9) Uani 1 1 d . . .
H21A H 0.2812 0.4452 0.1989 0.039 Uiso 1 1 calc R . .
C22 C 0.2405(3) 0.5736(4) 0.1438(3) 0.0376(10) Uani 1 1 d . . .
H22A H 0.1723 0.5571 0.1223 0.045 Uiso 1 1 calc R . .
C23 C 0.2749(3) 0.6643(3) 0.1299(3) 0.0339(9) Uani 1 1 d . . .
H23A H 0.2295 0.7101 0.1007 0.041 Uiso 1 1 calc R . .
C24 C 0.3751(3) 0.6888(3) 0.1584(3) 0.0279(8) Uani 1 1 d . . .
C25 C 0.4721(3) 0.4585(3) 0.2809(3) 0.0263(8) Uani 1 1 d . . .
H25A H 0.5446 0.4747 0.2773 0.032 Uiso 1 1 calc R . .
C26 C 0.4536(4) 0.4695(3) 0.3822(3) 0.0409(11) Uani 1 1 d . . .
H26A H 0.4631 0.5356 0.4009 0.061 Uiso 1 1 calc R . .
H26B H 0.5016 0.4299 0.4217 0.061 Uiso 1 1 calc R . .
H26C H 0.3842 0.4500 0.3885 0.061 Uiso 1 1 calc R . .
C27 C 0.4568(3) 0.3547(3) 0.2535(3) 0.0312(9) Uani 1 1 d . . .
H27A H 0.4683 0.3464 0.1891 0.047 Uiso 1 1 calc R . .
H27B H 0.3874 0.3356 0.2603 0.047 Uiso 1 1 calc R . .
H27C H 0.5048 0.3156 0.2935 0.047 Uiso 1 1 calc R . .
C28 C 0.4094(3) 0.7906(3) 0.1459(3) 0.0325(9) Uani 1 1 d . . .
H28A H 0.4828 0.7938 0.1713 0.039 Uiso 1 1 calc R . .
C29 C 0.4005(5) 0.8237(3) 0.0448(4) 0.0550(14) Uani 1 1 d . . .
H29A H 0.4237 0.8892 0.0428 0.083 Uiso 1 1 calc R . .
H29B H 0.3297 0.8197 0.0167 0.083 Uiso 1 1 calc R . .
H29C H 0.4425 0.7834 0.0107 0.083 Uiso 1 1 calc R . .
C30 C 0.3543(4) 0.8578(4) 0.2023(4) 0.0549(15) Uani 1 1 d . . .
H30A H 0.3606 0.8358 0.2664 0.082 Uiso 1 1 calc R . .
H30B H 0.2825 0.8603 0.1767 0.082 Uiso 1 1 calc R . .
H30C H 0.3840 0.9209 0.2004 0.082 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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
_geom_angle_publ_flag
C1 Pb1 Br1 91.23(8) . . ?
C1 Pb1 Br1 109.64(9) . 3_665 ?
Br1 Pb1 Br1 89.014(10) . 3_665 ?
Pb1 Br1 Pb1 90.986(10) . 3_665 ?
C2 C1 C6 119.5(3) . . ?
C2 C1 Pb1 109.0(2) . . ?
C6 C1 Pb1 131.4(3) . . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 C7 120.6(3) . . ?
C1 C2 C7 118.5(3) . . ?
C4 C3 C2 119.4(4) . . ?
C3 C4 C5 120.6(3) . . ?
C4 C5 C6 121.2(4) . . ?
C5 C6 C1 118.4(3) . . ?
C5 C6 C19 120.0(3) . . ?
C1 C6 C19 121.2(3) . . ?
C8 C7 C12 119.7(4) . . ?
C8 C7 C2 119.6(3) . . ?
C12 C7 C2 120.7(3) . . ?
C9 C8 C7 119.0(4) . . ?
C9 C8 C13 119.6(4) . . ?
C7 C8 C13 121.3(3) . . ?
C10 C9 C8 121.0(4) . . ?
C9 C10 C11 120.2(4) . . ?
C10 C11 C12 121.5(4) . . ?
C11 C12 C7 118.5(4) . . ?
C11 C12 C16 120.4(4) . . ?
C7 C12 C16 121.0(4) . . ?
C8 C13 C14 113.1(3) . . ?
C8 C13 C15 109.9(3) . . ?
C14 C13 C15 110.0(3) . . ?
C12 C16 C18 111.1(3) . . ?
C12 C16 C17 111.8(4) . . ?
C18 C16 C17 109.2(3) . . ?
C20 C19 C24 120.8(4) . . ?
C20 C19 C6 121.5(3) . . ?
C24 C19 C6 117.7(3) . . ?
C21 C20 C19 118.2(4) . . ?
C21 C20 C25 120.0(4) . . ?
C19 C20 C25 121.6(3) . . ?
C20 C21 C22 121.2(4) . . ?
C23 C22 C21 120.1(4) . . ?
C24 C23 C22 120.7(4) . . ?
C23 C24 C19 118.9(4) . . ?
C23 C24 C28 119.3(4) . . ?
C19 C24 C28 121.7(3) . . ?
C20 C25 C27 115.4(3) . . ?
C20 C25 C26 109.6(3) . . ?
C27 C25 C26 108.4(3) . . ?
C30 C28 C24 110.9(4) . . ?
C30 C28 C29 110.4(4) . . ?
C24 C28 C29 114.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 C1 2.322(3) . ?
Pb1 Br1 2.8125(5) . ?
Pb1 Br1 3.0346(5) 3_665 ?
Br1 Pb1 3.0346(5) 3_665 ?
C1 C2 1.404(5) . ?
C1 C6 1.408(5) . ?
C2 C3 1.392(5) . ?
C2 C7 1.515(5) . ?
C3 C4 1.377(6) . ?
C4 C5 1.385(6) . ?
C5 C6 1.401(5) . ?
C6 C19 1.503(5) . ?
C7 C8 1.411(5) . ?
C7 C12 1.422(5) . ?
C8 C9 1.400(6) . ?
C8 C13 1.520(5) . ?
C9 C10 1.372(6) . ?
C10 C11 1.377(7) . ?
C11 C12 1.393(6) . ?
C12 C16 1.523(6) . ?
C13 C14 1.528(5) . ?
C13 C15 1.538(6) . ?
C16 C18 1.526(6) . ?
C16 C17 1.549(6) . ?
C19 C20 1.414(6) . ?
C19 C24 1.416(5) . ?
C20 C21 1.392(6) . ?
C20 C25 1.527(5) . ?
C21 C22 1.394(6) . ?
C22 C23 1.389(7) . ?
C23 C24 1.389(6) . ?
C24 C28 1.532(6) . ?
C25 C27 1.532(6) . ?
C25 C26 1.541(5) . ?
C28 C30 1.511(6) . ?
C28 C29 1.540(6) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Pb1 Br1 Pb1 109.63(9) . . . 3_665 ?
Br1 Pb1 Br1 Pb1 0.0 3_665 . . 3_665 ?
Br1 Pb1 C1 C2 109.0(2) . . . . ?
Br1 Pb1 C1 C2 -161.6(2) 3_665 . . . ?
Br1 Pb1 C1 C6 -68.6(3) . . . . ?
Br1 Pb1 C1 C6 20.8(3) 3_665 . . . ?
C6 C1 C2 C3 -0.4(5) . . . . ?
Pb1 C1 C2 C3 -178.3(3) . . . . ?
C6 C1 C2 C7 179.5(3) . . . . ?
Pb1 C1 C2 C7 1.5(4) . . . . ?
C1 C2 C3 C4 1.4(5) . . . . ?
C7 C2 C3 C4 -178.4(3) . . . . ?
C2 C3 C4 C5 -0.8(5) . . . . ?
C3 C4 C5 C6 -0.9(6) . . . . ?
C4 C5 C6 C1 1.9(5) . . . . ?
C4 C5 C6 C19 -171.0(3) . . . . ?
C2 C1 C6 C5 -1.3(5) . . . . ?
Pb1 C1 C6 C5 176.2(3) . . . . ?
C2 C1 C6 C19 171.5(3) . . . . ?
Pb1 C1 C6 C19 -11.1(5) . . . . ?
C3 C2 C7 C8 82.3(4) . . . . ?
C1 C2 C7 C8 -97.5(4) . . . . ?
C3 C2 C7 C12 -100.1(4) . . . . ?
C1 C2 C7 C12 80.1(4) . . . . ?
C12 C7 C8 C9 -1.0(5) . . . . ?
C2 C7 C8 C9 176.6(3) . . . . ?
C12 C7 C8 C13 178.2(3) . . . . ?
C2 C7 C8 C13 -4.2(5) . . . . ?
C7 C8 C9 C10 0.8(6) . . . . ?
C13 C8 C9 C10 -178.4(4) . . . . ?
C8 C9 C10 C11 -0.4(7) . . . . ?
C9 C10 C11 C12 0.2(7) . . . . ?
C10 C11 C12 C7 -0.4(6) . . . . ?
C10 C11 C12 C16 178.4(4) . . . . ?
C8 C7 C12 C11 0.8(5) . . . . ?
C2 C7 C12 C11 -176.8(3) . . . . ?
C8 C7 C12 C16 -178.0(3) . . . . ?
C2 C7 C12 C16 4.4(5) . . . . ?
C9 C8 C13 C14 -37.6(5) . . . . ?
C7 C8 C13 C14 143.2(3) . . . . ?
C9 C8 C13 C15 85.7(4) . . . . ?
C7 C8 C13 C15 -93.5(4) . . . . ?
C11 C12 C16 C18 -82.5(5) . . . . ?
C7 C12 C16 C18 96.3(4) . . . . ?
C11 C12 C16 C17 39.8(5) . . . . ?
C7 C12 C16 C17 -141.4(4) . . . . ?
C5 C6 C19 C20 -82.7(4) . . . . ?
C1 C6 C19 C20 104.7(4) . . . . ?
C5 C6 C19 C24 95.2(4) . . . . ?
C1 C6 C19 C24 -77.5(4) . . . . ?
C24 C19 C20 C21 4.2(5) . . . . ?
C6 C19 C20 C21 -178.1(3) . . . . ?
C24 C19 C20 C25 -170.3(3) . . . . ?
C6 C19 C20 C25 7.4(5) . . . . ?
C19 C20 C21 C22 -2.4(6) . . . . ?
C25 C20 C21 C22 172.2(4) . . . . ?
C20 C21 C22 C23 -0.6(6) . . . . ?
C21 C22 C23 C24 2.0(6) . . . . ?
C22 C23 C24 C19 -0.3(6) . . . . ?
C22 C23 C24 C28 -177.2(4) . . . . ?
C20 C19 C24 C23 -2.9(5) . . . . ?
C6 C19 C24 C23 179.3(3) . . . . ?
C20 C19 C24 C28 174.0(3) . . . . ?
C6 C19 C24 C28 -3.8(5) . . . . ?
C21 C20 C25 C27 39.4(5) . . . . ?
C19 C20 C25 C27 -146.2(4) . . . . ?
C21 C20 C25 C26 -83.3(5) . . . . ?
C19 C20 C25 C26 91.1(4) . . . . ?
C23 C24 C28 C30 63.0(5) . . . . ?
C19 C24 C28 C30 -113.9(4) . . . . ?
C23 C24 C28 C29 -62.8(5) . . . . ?
C19 C24 C28 C29 120.4(4) . . . . ?
