#------------------------------------------------------------------------------
#$Date: 2017-10-13 08:09:21 +0200 (vie 13 de oct de 2017) $
#$Revision: 201973 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/22/2202247.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2202247
loop_
_publ_author_name
'Holger Fleischer'
'Simon Parsons'
'Colin R. Pulham'
_publ_section_title
;
 Tetramethyllead(IV) at 150K
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m11
_journal_page_last               m13
_journal_paper_doi               10.1107/S1600536802022201
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Pb (C1 H3)4]'
_chemical_formula_moiety         'C4 H12 Pb1'
_chemical_formula_sum            'C4 H12 Pb'
_chemical_formula_weight         267.34
_chemical_melting_point          243
_chemical_name_systematic
;
Tetramethyl lead
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.1725(6)
_cell_length_b                   11.1725(6)
_cell_length_c                   11.1725(6)
_cell_measurement_reflns_used    3546
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      3
_cell_volume                     1394.60(13)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT
;
_computing_molecular_graphics
;
CAMERON (Watkin et al., 1996)
;
_computing_publication_material
;
CRYSTALS
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al., 2001)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 1997)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type
;
Bruker SMART APEX CCD
;
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7703
_diffrn_reflns_theta_full        28.1
_diffrn_reflns_theta_max         28.6
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.07
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[SADABS (Sheldrick, 2002) based on the method of Blessing (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             944.00
_exptl_crystal_size_max          3.00
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_size_rad          0.20
_refine_diff_density_max         1.55
_refine_diff_density_min         -1.84
_refine_ls_extinction_coef       139.(12)
_refine_ls_extinction_method     'Larson (1970), equation 22'
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         577
_refine_ls_R_factor_all          0.048
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max          <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Tukey and Prince (Carruthers & Watkin, 1979)
W = [weight][1-(deltaF/6\sF)^2]^ where
[weight] is given by a five-term Chebychev polynomial
with coefficients: 96.4 162. 107. 51.2 13.7
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.121
_refine_ls_wR_factor_gt          0.094
_refine_ls_wR_factor_ref         0.105
_reflns_number_gt                375
_reflns_number_total             586
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ya6144.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     ' -P 2ac 2ab 3'
_cod_original_formula_sum        'C4 H12 Pb1'
_cod_database_code               2202247
_cod_database_fobs_code          2202247
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
y,z,x
-y,-z,-x
z,x,y
-z,-x,-y
x+1/2,y,-z+1/2
-x+1/2,-y,z+1/2
y+1/2,z,-x+1/2
-y+1/2,-z,x+1/2
z+1/2,x,-y+1/2
-z+1/2,-x,y+1/2
y+1/2,-z+1/2,-x
-y+1/2,z+1/2,x
z+1/2,-x+1/2,-y
-z+1/2,x+1/2,y
-z,x+1/2,-y+1/2
z,-x+1/2,y+1/2
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2
-y,z+1/2,-x+1/2
y,-z+1/2,x+1/2
x+1/2,-y+1/2,-z
-x+1/2,y+1/2,z
loop_
_atom_site_label
_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_type_symbol
Pb1 0.872030(14) 0.372030(14) 0.127970(14) 0.0145 Uani 1.0000 Pb
C1 0.7586(8) 0.2586(8) 0.2414(8) 0.0258 Uani 1.0000 C
C2 0.9865(8) 0.2561(6) 0.0148(5) 0.0224 Uani 1.0000 C
H11 0.7071 0.3109 0.2921 0.0315 Uiso 1.0000 H
H21 1.0390 0.3065 -0.0370 0.0254 Uiso 1.0000 H
H22 1.0382 0.2043 0.0675 0.0254 Uiso 1.0000 H
H23 0.9353 0.2035 -0.0363 0.0254 Uiso 1.0000 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pb1 0.0145(3) 0.0145(3) 0.0145(3) -0.00001(6) 0.00001(6) 0.00001(6)
C1 0.026(2) 0.026(2) 0.026(2) -0.002(3) 0.002(3) 0.002(3)
C2 0.027(3) 0.018(3) 0.021(2) 0.003(2) 0.005(3) -0.007(2)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C   ' 0.0033 0.0016 International_Tables_Vol_IV_Table_2.2B
'H   ' 0.0000 0.0000 International_Tables_Vol_IV_Table_2.2B
'Pb  ' -3.3944 10.1111 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 Pb1 C1 . 108.96(16) yes
C2 Pb1 C2 13_556 109.98(16) yes
Pb1 C2 H21 . 109.906 no
Pb1 C2 H22 . 109.458 no
H21 C2 H22 . 108.993 no
Pb1 C2 H23 . 109.858 no
H21 C2 H23 . 109.669 no
H22 C2 H23 . 108.937 no
Pb1 C1 H11 . 108.908 no
H11 C1 H11 13_556 110.029 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 C1 . . 2.194(15) yes
Pb1 C2 . . 2.216(7) yes
C2 H21 . . 0.998 no
C2 H22 . . 1.008 no
C2 H23 . . 0.999 no
C1 H11 . . 0.997 no
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 6154
