#------------------------------------------------------------------------------
#$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $
#$Revision: 19 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1100712.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_1100712
_publ_requested_journal          'Inorganic Chemistry'
loop_
_publ_author_name
'Leslie W. Pineda'
'Vojtech Jancik'
'Herbert W. Roesky*'
'Regine Herbst-Irmer'
_chemical_formula_moiety         LGe(m-O)ZrCp2Me
_chemical_formula_sum            'C40 H54 Ge N2 O Zr'
_chemical_formula_weight         742.66
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           TRICLINIC
_symmetry_space_group_name_H-M   P-1
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   9.444(1)
_cell_length_b                   10.522(1)
_cell_length_c                   19.750(1)
_cell_angle_alpha                88.64(1)
_cell_angle_beta                 89.60(1)
_cell_angle_gamma                67.44(1)
_cell_volume                     1812(1)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5044
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      58.96
_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    3.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7137
_exptl_absorpt_correction_T_max  0.8992
_exptl_absorpt_process_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_detector_area_resol_mean 5.602
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14140
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         58.96
_reflns_number_total             5044
_reflns_number_gt                4879
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+2.5234P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00036(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5044
_refine_ls_number_parameters     421
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0728
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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
Zr1 Zr -0.14748(3) 0.92344(2) 0.239776(11) 0.02037(10) Uani 1 1 d . . .
Ge1 Ge 0.26023(3) 0.78468(3) 0.251684(14) 0.01964(11) Uani 1 1 d . . .
N1 N 0.3612(2) 0.6265(2) 0.18811(10) 0.0194(5) Uani 1 1 d . . .
O1 O 0.0661(2) 0.79553(19) 0.24598(9) 0.0242(4) Uani 1 1 d . . .
C1 C 0.5647(3) 0.4803(3) 0.39116(13) 0.0236(6) Uani 1 1 d . . .
H1A H 0.4913 0.4973 0.4285 0.035 Uiso 0.50 1 calc PR . .
H1B H 0.6446 0.5139 0.4030 0.035 Uiso 0.50 1 calc PR . .
H1C H 0.6117 0.3813 0.3830 0.035 Uiso 0.50 1 calc PR . .
H1D H 0.6737 0.4311 0.3812 0.035 Uiso 0.50 1 calc PR . .
H1E H 0.5204 0.4144 0.4067 0.035 Uiso 0.50 1 calc PR . .
H1F H 0.5533 0.5470 0.4266 0.035 Uiso 0.50 1 calc PR . .
N2 N 0.3370(2) 0.6419(2) 0.33005(10) 0.0183(5) Uani 1 1 d . . .
C2 C 0.4822(3) 0.5550(3) 0.32784(13) 0.0187(6) Uani 1 1 d . . .
C3 C 0.5663(3) 0.5267(3) 0.26735(13) 0.0194(6) Uani 1 1 d . . .
H3A H 0.664(4) 0.476(3) 0.2714(15) 0.023 Uiso 1 1 d . . .
C4 C 0.5076(3) 0.5491(3) 0.20125(13) 0.0189(6) Uani 1 1 d . . .
C5 C 0.6165(3) 0.4840(3) 0.14429(13) 0.0252(6) Uani 1 1 d . . .
H5A H 0.5629 0.4545 0.1095 0.038 Uiso 1 1 calc R . .
H5B H 0.7032 0.4041 0.1619 0.038 Uiso 1 1 calc R . .
H5C H 0.6543 0.5513 0.1244 0.038 Uiso 1 1 calc R . .
C6 C 0.2942(3) 0.6236(3) 0.12282(13) 0.0208(6) Uani 1 1 d . . .
C7 C 0.2944(3) 0.7176(3) 0.07119(13) 0.0234(6) Uani 1 1 d . . .
C8 C 0.2188(3) 0.7160(3) 0.01059(14) 0.0291(7) Uani 1 1 d . . .
H8A H 0.2135 0.7811 -0.0244 0.035 Uiso 1 1 calc R . .
C9 C 0.1522(3) 0.6227(3) 0.00064(14) 0.0307(7) Uani 1 1 d . . .
H9A H 0.1027 0.6231 -0.0411 0.037 Uiso 1 1 calc R . .
C10 C 0.1570(3) 0.5280(3) 0.05131(14) 0.0270(6) Uani 1 1 d . . .
H10A H 0.1129 0.4622 0.0434 0.032 Uiso 1 1 calc R . .
C11 C 0.2256(3) 0.5274(3) 0.11385(13) 0.0228(6) Uani 1 1 d . . .
C12 C 0.2260(3) 0.4253(3) 0.16999(14) 0.0255(6) Uani 1 1 d . . .
H12A H 0.2120 0.4739 0.2139 0.031 Uiso 1 1 calc R . .
C13 C 0.0969(4) 0.3718(3) 0.16389(16) 0.0351(7) Uani 1 1 d . . .
H13A H 0.0001 0.4491 0.1539 0.053 Uiso 1 1 calc R . .
H13B H 0.0874 0.3265 0.2066 0.053 Uiso 1 1 calc R . .
H13C H 0.1206 0.3057 0.1273 0.053 Uiso 1 1 calc R . .
C14 C 0.3777(4) 0.2999(3) 0.17425(16) 0.0347(7) Uani 1 1 d . . .
H14A H 0.4616 0.3302 0.1833 0.052 Uiso 1 1 calc R . .
H14B H 0.3963 0.2515 0.1313 0.052 Uiso 1 1 calc R . .
H14C H 0.3721 0.2376 0.2110 0.052 Uiso 1 1 calc R . .
C15 C 0.3790(3) 0.8139(3) 0.07656(13) 0.0261(6) Uani 1 1 d . . .
H15A H 0.4360 0.7931 0.1206 0.031 Uiso 1 1 calc R . .
C16 C 0.4972(4) 0.7878(3) 0.01904(14) 0.0326(7) Uani 1 1 d . . .
H16A H 0.5665 0.6906 0.0201 0.049 Uiso 1 1 calc R . .
H16B H 0.5565 0.8454 0.0251 0.049 Uiso 1 1 calc R . .
H16C H 0.4437 0.8108 -0.0246 0.049 Uiso 1 1 calc R . .
C17 C 0.2706(4) 0.9653(3) 0.07593(15) 0.0352(7) Uani 1 1 d . . .
H17A H 0.2036 0.9830 0.1157 0.053 Uiso 1 1 calc R . .
H17B H 0.2081 0.9867 0.0346 0.053 Uiso 1 1 calc R . .
H17C H 0.3306 1.0234 0.0771 0.053 Uiso 1 1 calc R . .
C18 C 0.2531(3) 0.6727(3) 0.39271(12) 0.0188(6) Uani 1 1 d . . .
C19 C 0.1388(3) 0.6193(3) 0.40480(13) 0.0205(6) Uani 1 1 d . . .
C20 C 0.0532(3) 0.6561(3) 0.46422(13) 0.0238(6) Uani 1 1 d . . .
H20A H -0.0239 0.6210 0.4735 0.029 Uiso 1 1 calc R . .
C21 C 0.0789(3) 0.7429(3) 0.50986(13) 0.0246(6) Uani 1 1 d . . .
H21A H 0.0199 0.7663 0.5502 0.029 Uiso 1 1 calc R . .
C22 C 0.1896(3) 0.7954(3) 0.49707(13) 0.0229(6) Uani 1 1 d . . .
H22A H 0.2060 0.8547 0.5288 0.027 Uiso 1 1 calc R . .
C23 C 0.2782(3) 0.7629(3) 0.43816(13) 0.0204(6) Uani 1 1 d . . .
C24 C 0.3941(3) 0.8291(3) 0.42555(13) 0.0235(6) Uani 1 1 d . . .
H24A H 0.4521 0.7896 0.3834 0.028 Uiso 1 1 calc R . .
C25 C 0.5098(4) 0.7984(3) 0.48390(14) 0.0318(7) Uani 1 1 d . . .
H25A H 0.5630 0.6986 0.4901 0.048 Uiso 1 1 calc R . .
H25B H 0.4555 0.8375 0.5257 0.048 Uiso 1 1 calc R . .
H25C H 0.5846 0.8396 0.4732 0.048 Uiso 1 1 calc R . .
C26 C 0.3116(4) 0.9850(3) 0.41394(15) 0.0324(7) Uani 1 1 d . . .
H26A H 0.2433 1.0029 0.3746 0.049 Uiso 1 1 calc R . .
H26B H 0.3875 1.0261 0.4056 0.049 Uiso 1 1 calc R . .
H26C H 0.2513 1.0256 0.4541 0.049 Uiso 1 1 calc R . .
C27 C 0.1125(3) 0.5234(3) 0.35456(13) 0.0235(6) Uani 1 1 d . . .
H27A H 0.1284 0.5554 0.3081 0.028 Uiso 1 1 calc R . .
C28 C -0.0500(3) 0.5243(3) 0.35706(15) 0.0295(7) Uani 1 1 d . . .
H28A H -0.1248 0.6190 0.3513 0.044 Uiso 1 1 calc R . .
H28B H -0.0664 0.4864 0.4009 0.044 Uiso 1 1 calc R . .
H28C H -0.0630 0.4681 0.3206 0.044 Uiso 1 1 calc R . .
C29 C 0.2294(3) 0.3752(3) 0.36466(15) 0.0306(7) Uani 1 1 d . . .
H29A H 0.3332 0.3728 0.3577 0.046 Uiso 1 1 calc R . .
H29B H 0.2090 0.3156 0.3320 0.046 Uiso 1 1 calc R . .
H29C H 0.2206 0.3425 0.4108 0.046 Uiso 1 1 calc R . .
C30 C -0.1172(4) 1.0793(3) 0.16446(16) 0.0363(7) Uani 1 1 d . . .
H30A H -0.0738 1.0333 0.1222 0.055 Uiso 1 1 calc R . .
H30B H -0.0478 1.1184 0.1837 0.055 Uiso 1 1 calc R . .
H30C H -0.2171 1.1532 0.1551 0.055 Uiso 1 1 calc R . .
C31 C -0.1727(4) 0.7859(4) 0.14037(16) 0.0402(8) Uani 1 1 d . . .
H31A H -0.0889 0.7532 0.1098 0.048 Uiso 1 1 calc R . .
C32 C -0.1926(4) 0.7177(3) 0.19842(17) 0.0396(8) Uani 1 1 d . . .
H32A H -0.1251 0.6293 0.2141 0.047 Uiso 1 1 calc R . .
C33 C -0.3286(4) 0.8008(3) 0.22983(18) 0.0419(8) Uani 1 1 d . . .
H33A H -0.3686 0.7797 0.2710 0.050 Uiso 1 1 calc R . .
C34 C -0.3957(4) 0.9210(3) 0.18977(18) 0.0399(8) Uani 1 1 d . . .
H34A H -0.4901 0.9950 0.1985 0.048 Uiso 1 1 calc R . .
C35 C -0.2990(4) 0.9124(4) 0.13487(17) 0.0431(9) Uani 1 1 d . . .
H35A H -0.3154 0.9801 0.0999 0.052 Uiso 1 1 calc R . .
C36 C -0.3495(4) 1.0635(3) 0.32486(15) 0.0383(8) Uani 1 1 d . . .
H36A H -0.4536 1.0763 0.3178 0.046 Uiso 1 1 calc R . .
C37 C -0.2798(4) 1.1505(3) 0.30176(15) 0.0360(8) Uani 1 1 d . . .
H37A H -0.3274 1.2324 0.2753 0.043 Uiso 1 1 calc R . .
C38 C -0.1256(4) 1.0965(3) 0.32432(15) 0.0344(7) Uani 1 1 d . . .
H38A H -0.0513 1.1353 0.3156 0.041 Uiso 1 1 calc R . .
C39 C -0.1023(4) 0.9754(3) 0.36177(14) 0.0315(7) Uani 1 1 d . . .
H39A H -0.0100 0.9187 0.3840 0.038 Uiso 1 1 calc R . .
C40 C -0.2389(4) 0.9524(3) 0.36081(14) 0.0352(7) Uani 1 1 d . . .
H40A H -0.2544 0.8758 0.3808 0.042 Uiso 1 1 calc R . .