#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:44:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178665 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/76/4077693.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_4077693
loop_
_publ_author_name
'Constantine, Steven P.'
'Cox, Hazel'
'Hitchcock, Peter B.'
'Lawless, Gerard A.'
_publ_section_title
;
 Parallel Metallocenes of Germanium, Tin, and Lead
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              317
_journal_paper_doi               10.1021/om990884z
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C30 H54 Ge Si2'
_chemical_formula_weight         543.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 92.25(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.207(4)
_cell_length_b                   8.781(4)
_cell_length_c                   13.844(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1604.3(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.1596
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4835
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.045
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.217
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         4659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      1.217
_refine_ls_R_factor_all          0.2088
_refine_ls_R_factor_obs          0.0839
_refine_ls_shift/esd_max         0.019
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0696P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2072
_refine_ls_wR_factor_obs         0.1549
_reflns_number_observed          1949
_reflns_number_total             4662
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990884z.cif
_cod_data_source_block           steven
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4077693
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ge Ge 0.0000 0.0000 0.0000 0.0435(2) Uani 1 d S .
M1 C 0.0026 0.2356 0.0565 0.000 Uiso 0.00 d P 1
Si Si -0.00490(12) 0.1188(2) 0.26600(10) 0.0514(4) Uani 1 d . 2
C1 C -0.0010(3) 0.1840(5) 0.1377(3) 0.0386(11) Uani 1 d . 2
C2 C 0.0873(4) 0.2174(5) 0.0866(4) 0.0496(13) Uani 1 d . 2
C3 C 0.0583(5) 0.2732(5) -0.0055(4) 0.0596(15) Uani 1 d . 2
C4 C -0.0469(5) 0.2789(5) -0.0117(3) 0.058(2) Uani 1 d . 2
C5 C -0.0845(4) 0.2241(5) 0.0753(4) 0.0469(12) Uani 1 d . 2
C6 C 0.1958(4) 0.1993(8) 0.1192(5) 0.089(2) Uani 1 d . 2
H6A H 0.2029(7) 0.1107(30) 0.1595(27) 0.134 Uiso 1 calc R 2
H6B H 0.2174(11) 0.2877(24) 0.1552(29) 0.134 Uiso 1 calc R 2
H6C H 0.2368(6) 0.1879(53) 0.0639(5) 0.134 Uiso 1 calc R 2
C7 C 0.1265(6) 0.3292(7) -0.0823(5) 0.107(3) Uani 1 d . 2
H7A H 0.0983(22) 0.3017(56) -0.1448(5) 0.161 Uiso 1 calc R 2
H7B H 0.1923(13) 0.2838(49) -0.0730(24) 0.161 Uiso 1 calc R 2
H7C H 0.1325(34) 0.4380(9) -0.0781(26) 0.161 Uiso 1 calc R 2
C8 C -0.1108(6) 0.3384(7) -0.0970(4) 0.100(2) Uani 1 d . 2
H8A H -0.0750(17) 0.3244(53) -0.1554(6) 0.150 Uiso 1 calc R 2
H8B H -0.1241(33) 0.4449(15) -0.0880(18) 0.150 Uiso 1 calc R 2
H8C H -0.1737(17) 0.2837(40) -0.1016(22) 0.150 Uiso 1 calc R 2
C9 C -0.1950(4) 0.2127(8) 0.0958(4) 0.084(2) Uani 1 d . 2
H9A H -0.2041(5) 0.2318(50) 0.1632(8) 0.126 Uiso 1 calc R 2
H9B H -0.2191(9) 0.1125(17) 0.0797(30) 0.126 Uiso 1 calc R 2
H9C H -0.2323(6) 0.2867(34) 0.0578(24) 0.126 Uiso 1 calc R 2
C10 C 0.1035(6) -0.0071(7) 0.3017(5) 0.099(2) Uani 1 d . 2
H10A H 0.0981(6) -0.0374(7) 0.3680(5) 0.149 Uiso 1 calc R 2
H10B H 0.1659(6) 0.0469(7) 0.2945(5) 0.149 Uiso 1 calc R 2
H10C H 0.1024(6) -0.0958(7) 0.2612(5) 0.149 Uiso 1 calc R 2
C11 C -0.1205(5) 0.0029(8) 0.2888(4) 0.097(2) Uani 1 d . 2
H11A H -0.1800(5) 0.0614(8) 0.2718(4) 0.145 Uiso 1 calc R 2
H11B H -0.1209(5) -0.0241(8) 0.3560(4) 0.145 Uiso 1 calc R 2
H11C H -0.1199(5) -0.0880(8) 0.2503(4) 0.145 Uiso 1 calc R 2
C12 C -0.0032(4) 0.2905(6) 0.3495(3) 0.0578(15) Uani 1 d . 2
C13 C -0.0942(5) 0.3915(7) 0.3278(5) 0.088(2) Uani 1 d . 2
H13A H -0.1552(5) 0.3337(7) 0.3345(5) 0.132 Uiso 1 calc R 2
H13B H -0.0918(5) 0.4294(7) 0.2628(5) 0.132 Uiso 1 calc R 2
H13C H -0.0933(5) 0.4755(7) 0.3722(5) 0.132 Uiso 1 calc R 2
C14 C 0.0920(5) 0.3853(7) 0.3380(5) 0.086(2) Uani 1 d . 2
H14A H 0.1507(5) 0.3232(7) 0.3515(5) 0.129 Uiso 1 calc R 2
H14B H 0.0920(5) 0.4694(7) 0.3822(5) 0.129 Uiso 1 calc R 2
H14C H 0.0934(5) 0.4229(7) 0.2730(5) 0.129 Uiso 1 calc R 2
C15 C -0.0078(6) 0.2357(9) 0.4554(4) 0.107(3) Uani 1 d . 2
H15A H 0.0493(6) 0.1712(9) 0.4707(4) 0.161 Uiso 1 calc R 2
H15B H -0.0693(6) 0.1798(9) 0.4634(4) 0.161 Uiso 1 calc R 2
H15C H -0.0061(6) 0.3223(9) 0.4978(4) 0.161 Uiso 1 calc R 2
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
C1 Ge C5 32.92(14)
C1 Ge C2 32.90(14)
C5 Ge C2 53.76(15)
C1 Ge C3 54.48(15)
C5 Ge C3 53.7(2)
C2 Ge C3 32.4(2)
C1 Ge C4 54.16(14)
C5 Ge C4 32.4(2)
C2 Ge C4 53.2(2)
C3 Ge C4 31.9(2)
C10 Si C1 112.6(3)
C10 Si C11 104.8(3)
C1 Si C11 112.3(3)
C10 Si C12 108.6(3)
C1 Si C12 109.6(2)
C11 Si C12 108.6(3)
C2 C1 C5 106.2(4)
C2 C1 Si 126.3(4)
C5 C1 Si 127.2(3)
C2 C1 Ge 74.0(2)
C5 C1 Ge 73.9(2)
Si C1 Ge 121.9(2)
C3 C2 C1 109.0(4)
C3 C2 C6 122.4(5)
C1 C2 C6 128.6(5)
C3 C2 Ge 74.2(3)
C1 C2 Ge 73.1(2)
C6 C2 Ge 118.7(4)
C4 C3 C2 107.7(5)
C4 C3 C7 124.8(5)
C2 C3 C7 127.3(6)
C4 C3 Ge 74.4(3)
C2 C3 Ge 73.4(3)
C7 C3 Ge 121.7(4)
C3 C4 C5 108.8(5)
C3 C4 C8 125.7(5)
C5 C4 C8 125.4(6)
C3 C4 Ge 73.7(3)
C5 C4 Ge 73.0(3)
C8 C4 Ge 120.7(3)
C4 C5 C1 108.3(4)
C4 C5 C9 124.4(5)
C1 C5 C9 127.3(5)
C4 C5 Ge 74.6(3)
C1 C5 Ge 73.2(2)
C9 C5 Ge 118.6(4)
C13 C12 C14 108.2(5)
C13 C12 C15 108.0(5)
C14 C12 C15 109.4(5)
C13 C12 Si 110.7(4)
C14 C12 Si 111.2(4)
C15 C12 Si 109.3(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ge M1 2.2111(9)
Ge C1 2.499(4)
Ge C5 2.509(4)
Ge C2 2.511(5)
Ge C3 2.521(5)
Ge C4 2.529(5)
Si C10 1.860(6)
Si C1 1.868(5)
Si C11 1.872(6)
Si C12 1.899(5)
C1 C2 1.419(6)
C1 C5 1.419(6)
C2 C3 1.405(7)
C2 C6 1.494(7)
C3 C4 1.389(7)
C3 C7 1.503(7)
C4 C5 1.405(7)
C4 C8 1.518(8)
C5 C9 1.501(7)
C12 C13 1.515(8)
C12 C14 1.521(8)
C12 C15 1.547(7)
