#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:11:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179743 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/39/7003908.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_7003908
loop_
_publ_author_name
'Jones, Cameron'
'Rose, Richard P.'
'Stasch, Andreas'
_publ_section_title
;
 Synthesis, characterisation and reactivity of germanium(ii) amidinate
 and guanidinate complexes
;
_journal_issue                   21
_journal_name_full               'Dalton Transactions'
_journal_page_first              2871
_journal_page_last               2878
_journal_paper_doi               10.1039/b801168k
_journal_year                    2008
_chemical_formula_sum            'C34 H43 Cl Ge N2 O5 W'
_chemical_formula_weight         851.59
_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                 101.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.592(2)
_cell_length_b                   16.684(3)
_cell_length_c                   21.013(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3636.6(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26171
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    4.100
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0335
_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)+(0.0304P)²+5.6010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                6361
_reflns_number_total             7377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801168k.txt
_cod_data_source_block           compound4
_cod_original_cell_volume        3636.6(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7003908
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
W1 W 0.267465(14) 0.106817(10) 0.080170(7) 0.02857(8) Uani 1 1 d . . .
Ge1 Ge 0.34839(3) 0.20917(2) 0.169669(17) 0.01933(10) Uani 1 1 d . . .
Cl1 Cl 0.19632(8) 0.29535(6) 0.18124(4) 0.0276(2) Uani 1 1 d . . .
O1 O 0.1227(4) 0.0260(3) 0.1819(2) 0.0753(12) Uani 1 1 d . . .
N1 N 0.5004(3) 0.27896(17) 0.18635(14) 0.0192(6) Uani 1 1 d . . .
C1 C 0.5276(3) 0.2632(2) 0.25080(16) 0.0180(7) Uani 1 1 d . A .
O2 O 0.0292(3) 0.2230(2) 0.03390(16) 0.0601(10) Uani 1 1 d . . .
N2 N 0.4388(3) 0.21069(17) 0.26175(13) 0.0176(6) Uani 1 1 d . . .
C2 C 0.6291(3) 0.3067(2) 0.30141(18) 0.0260(8) Uani 1 1 d . . .
O3 O 0.1264(4) -0.0061(3) -0.03201(19) 0.0741(13) Uani 1 1 d . . .
C3 C 0.5741(8) 0.3963(4) 0.2943(4) 0.037(2) Uani 0.586(7) 1 d P A 1
H3A H 0.6299 0.4312 0.3254 0.055 Uiso 0.586(7) 1 calc PR A 1
H3B H 0.4866 0.3970 0.3030 0.055 Uiso 0.586(7) 1 calc PR A 1
H3C H 0.5721 0.4156 0.2500 0.055 Uiso 0.586(7) 1 calc PR A 1
O4 O 0.4186(4) 0.1988(3) -0.01417(18) 0.0748(13) Uani 1 1 d . . .
C4 C 0.7641(7) 0.3091(6) 0.2853(4) 0.037(2) Uani 0.586(7) 1 d P A 1
H4A H 0.7583 0.3305 0.2414 0.056 Uiso 0.586(7) 1 calc PR A 1
H4B H 0.7999 0.2547 0.2875 0.056 Uiso 0.586(7) 1 calc PR A 1
H4C H 0.8204 0.3435 0.3167 0.056 Uiso 0.586(7) 1 calc PR A 1
O5 O 0.4951(3) -0.0211(2) 0.10815(19) 0.0559(9) Uani 1 1 d . . .
C5 C 0.6386(7) 0.2803(5) 0.3698(3) 0.035(2) Uani 0.586(7) 1 d P A 1
H5A H 0.7059 0.3113 0.3983 0.052 Uiso 0.586(7) 1 calc PR A 1
H5B H 0.6606 0.2232 0.3736 0.052 Uiso 0.586(7) 1 calc PR A 1
H5C H 0.5558 0.2890 0.3827 0.052 Uiso 0.586(7) 1 calc PR A 1
C6 C 0.5728(3) 0.3180(2) 0.14472(16) 0.0216(7) Uani 1 1 d . . .
C7 C 0.5273(4) 0.3912(2) 0.11539(18) 0.0243(8) Uani 1 1 d . . .
C8 C 0.5944(4) 0.4266(2) 0.0727(2) 0.0320(9) Uani 1 1 d . . .
H8 H 0.5656 0.4766 0.0535 0.038 Uiso 1 1 calc R . .
C9 C 0.7028(4) 0.3909(2) 0.0574(2) 0.0356(10) Uani 1 1 d . . .
H9 H 0.7473 0.4161 0.0279 0.043 Uiso 1 1 calc R . .
C10 C 0.7456(4) 0.3182(3) 0.08549(19) 0.0329(9) Uani 1 1 d . . .
H10 H 0.8199 0.2939 0.0750 0.039 Uiso 1 1 calc R . .
C11 C 0.6820(3) 0.2798(2) 0.12878(18) 0.0255(8) Uani 1 1 d . . .
C12 C 0.4047(4) 0.4307(2) 0.12750(19) 0.0277(8) Uani 1 1 d . . .
H12 H 0.3803 0.4040 0.1659 0.033 Uiso 1 1 calc R . .
C13 C 0.2952(4) 0.4155(3) 0.0674(2) 0.0433(11) Uani 1 1 d . . .
H13A H 0.3167 0.4417 0.0292 0.065 Uiso 1 1 calc R . .
H13B H 0.2141 0.4375 0.0756 0.065 Uiso 1 1 calc R . .
H13C H 0.2855 0.3577 0.0595 0.065 Uiso 1 1 calc R . .
C14 C 0.4187(5) 0.5204(3) 0.1417(2) 0.0438(11) Uani 1 1 d . . .
H14A H 0.4878 0.5292 0.1797 0.066 Uiso 1 1 calc R . .
H14B H 0.3374 0.5414 0.1504 0.066 Uiso 1 1 calc R . .
H14C H 0.4397 0.5481 0.1040 0.066 Uiso 1 1 calc R . .
C15 C 0.7310(4) 0.1976(2) 0.1551(2) 0.0306(9) Uani 1 1 d . . .
H15 H 0.6876 0.1837 0.1918 0.037 Uiso 1 1 calc R . .
C16 C 0.8769(4) 0.1953(3) 0.1808(3) 0.0566(14) Uani 1 1 d . . .
H16A H 0.9007 0.1441 0.2028 0.085 Uiso 1 1 calc R . .
H16B H 0.9021 0.2394 0.2115 0.085 Uiso 1 1 calc R . .
H16C H 0.9213 0.2009 0.1444 0.085 Uiso 1 1 calc R . .
C17 C 0.6961(5) 0.1346(3) 0.1032(3) 0.0505(13) Uani 1 1 d . . .
H17A H 0.7391 0.1466 0.0671 0.076 Uiso 1 1 calc R . .
H17B H 0.6025 0.1343 0.0873 0.076 Uiso 1 1 calc R . .
H17C H 0.7241 0.0819 0.1214 0.076 Uiso 1 1 calc R . .
C18 C 0.4299(3) 0.1685(2) 0.32063(17) 0.0198(7) Uani 1 1 d . . .
C19 C 0.3605(3) 0.2002(2) 0.36462(18) 0.0224(8) Uani 1 1 d . . .
C20 C 0.3676(4) 0.1606(2) 0.42353(18) 0.0280(8) Uani 1 1 d . . .
H20 H 0.3224 0.1817 0.4545 0.034 Uiso 1 1 calc R . .
C21 C 0.4394(4) 0.0911(3) 0.4378(2) 0.0344(10) Uani 1 1 d . . .
H21 H 0.4479 0.0669 0.4794 0.041 Uiso 1 1 calc R . .
C22 C 0.4982(4) 0.0572(3) 0.3916(2) 0.0338(9) Uani 1 1 d . . .
H22 H 0.5436 0.0081 0.4010 0.041 Uiso 1 1 calc R . .
C23 C 0.4924(4) 0.0937(2) 0.33142(19) 0.0256(8) Uani 1 1 d . . .
C24 C 0.2741(3) 0.2735(2) 0.35042(19) 0.0268(8) Uani 1 1 d . . .
H24 H 0.2950 0.3013 0.3117 0.032 Uiso 1 1 calc R . .
C25 C 0.2909(5) 0.3340(3) 0.4063(2) 0.0503(13) Uani 1 1 d . . .
H25A H 0.2635 0.3096 0.4437 0.075 Uiso 1 1 calc R . .
H25B H 0.2382 0.3816 0.3923 0.075 Uiso 1 1 calc R . .
H25C H 0.3818 0.3496 0.4186 0.075 Uiso 1 1 calc R . .
C26 C 0.1332(4) 0.2464(3) 0.3330(2) 0.0455(12) Uani 1 1 d . . .
H26A H 0.1224 0.2080 0.2970 0.068 Uiso 1 1 calc R . .
H26B H 0.0776 0.2930 0.3200 0.068 Uiso 1 1 calc R . .
H26C H 0.1094 0.2208 0.3708 0.068 Uiso 1 1 calc R . .
C27 C 0.5494(4) 0.0512(2) 0.2797(2) 0.0337(9) Uani 1 1 d . . .
H27 H 0.5248 0.0824 0.2384 0.040 Uiso 1 1 calc R . .
C28 C 0.4923(7) -0.0323(3) 0.2674(3) 0.0707(18) Uani 1 1 d . . .
H28A H 0.5189 -0.0651 0.3065 0.106 Uiso 1 1 calc R . .
H28B H 0.5231 -0.0569 0.2311 0.106 Uiso 1 1 calc R . .
H28C H 0.3980 -0.0286 0.2568 0.106 Uiso 1 1 calc R . .
C29 C 0.6967(5) 0.0476(5) 0.2975(3) 0.081(2) Uani 1 1 d . . .
H29A H 0.7314 0.1020 0.3052 0.122 Uiso 1 1 calc R . .
H29B H 0.7297 0.0231 0.2617 0.122 Uiso 1 1 calc R . .
H29C H 0.7235 0.0154 0.3369 0.122 Uiso 1 1 calc R . .
C30 C 0.1758(4) 0.0537(3) 0.1451(2) 0.0434(11) Uani 1 1 d . . .
C31 C 0.1156(4) 0.1828(3) 0.0516(2) 0.0398(11) Uani 1 1 d . . .
C32 C 0.1801(4) 0.0341(3) 0.0090(2) 0.0495(13) Uani 1 1 d . . .
C33 C 0.3635(5) 0.1649(3) 0.0197(2) 0.0470(12) Uani 1 1 d . . .
C34 C 0.4146(4) 0.0264(3) 0.1001(2) 0.0366(10) Uani 1 1 d . . .
C5A C 0.5709(10) 0.3396(6) 0.3566(5) 0.033(3) Uani 0.414(7) 1 d P A 2
H5A1 H 0.6372 0.3683 0.3874 0.049 Uiso 0.414(7) 1 calc PR A 2
H5A2 H 0.5374 0.2952 0.3789 0.049 Uiso 0.414(7) 1 calc PR A 2
H5A3 H 0.5004 0.3764 0.3389 0.049 Uiso 0.414(7) 1 calc PR A 2
C4A C 0.7315(9) 0.2371(7) 0.3359(5) 0.038(3) Uani 0.414(7) 1 d P A 2
H4A1 H 0.7650 0.2080 0.3024 0.056 Uiso 0.414(7) 1 calc PR A 2
H4A2 H 0.6872 0.1996 0.3598 0.056 Uiso 0.414(7) 1 calc PR A 2
H4A3 H 0.8031 0.2625 0.3660 0.056 Uiso 0.414(7) 1 calc PR A 2
C3A C 0.7052(11) 0.3675(7) 0.2763(5) 0.038(3) Uani 0.414(7) 1 d P A 2
H3A1 H 0.7652 0.3924 0.3125 0.057 Uiso 0.414(7) 1 calc PR A 2
H3A2 H 0.6476 0.4085 0.2529 0.057 Uiso 0.414(7) 1 calc PR A 2
H3A3 H 0.7538 0.3424 0.2466 0.057 Uiso 0.414(7) 1 calc PR A 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
C32 W1 C33 92.1(2) . . ?
C32 W1 C30 91.5(2) . . ?
C33 W1 C30 176.41(19) . . ?
C32 W1 C34 88.47(18) . . ?
C33 W1 C34 89.05(18) . . ?
C30 W1 C34 91.39(19) . . ?
C32 W1 C31 86.50(18) . . ?
C33 W1 C31 89.15(19) . . ?
C30 W1 C31 90.72(19) . . ?
C34 W1 C31 174.59(16) . . ?
C32 W1 Ge1 172.00(14) . . ?
C33 W1 Ge1 90.32(15) . . ?
C30 W1 Ge1 86.08(13) . . ?
C34 W1 Ge1 99.21(12) . . ?
C31 W1 Ge1 85.90(12) . . ?
N1 Ge1 N2 66.42(12) . . ?
N1 Ge1 Cl1 100.64(9) . . ?
N2 Ge1 Cl1 95.93(9) . . ?
N1 Ge1 W1 132.01(9) . . ?
N2 Ge1 W1 138.78(8) . . ?
Cl1 Ge1 W1 111.86(3) . . ?
C1 N1 C6 132.0(3) . . ?
C1 N1 Ge1 93.7(2) . . ?
C6 N1 Ge1 133.1(2) . . ?
N2 C1 N1 106.5(3) . . ?
N2 C1 C2 127.5(3) . . ?
N1 C1 C2 125.5(3) . . ?
C1 N2 C18 129.5(3) . . ?
C1 N2 Ge1 93.3(2) . . ?
C18 N2 Ge1 136.9(2) . . ?
C3A C2 C5 128.4(5) . . ?
C3A C2 C5A 111.3(7) . . ?
C5 C2 C5A 47.9(5) . . ?
C3A C2 C1 116.0(5) . . ?
C5 C2 C1 115.6(4) . . ?
C5A C2 C1 111.4(4) . . ?
C3A C2 C4 45.2(6) . . ?
C5 C2 C4 109.7(5) . . ?
C5A C2 C4 134.3(5) . . ?
C1 C2 C4 114.4(4) . . ?
C3A C2 C3 62.2(6) . . ?
C5 C2 C3 108.6(5) . . ?
C5A C2 C3 62.5(5) . . ?
C1 C2 C3 100.8(3) . . ?
C4 C2 C3 107.0(5) . . ?
C3A C2 C4A 106.6(7) . . ?
C5 C2 C4A 57.2(5) . . ?
C5A C2 C4A 104.5(6) . . ?
C1 C2 C4A 106.1(4) . . ?
C4 C2 C4A 63.7(5) . . ?
C3 C2 C4A 153.0(5) . . ?
C7 C6 C11 120.6(3) . . ?
C7 C6 N1 118.9(3) . . ?
C11 C6 N1 120.2(3) . . ?
C8 C7 C6 118.6(4) . . ?
C8 C7 C12 119.3(3) . . ?
C6 C7 C12 122.1(3) . . ?
C7 C8 C9 121.6(4) . . ?
C10 C9 C8 119.5(4) . . ?
C9 C10 C11 121.4(4) . . ?
C10 C11 C6 118.3(4) . . ?
C10 C11 C15 118.4(3) . . ?
C6 C11 C15 123.3(3) . . ?
C7 C12 C14 113.9(3) . . ?
C7 C12 C13 108.4(3) . . ?
C14 C12 C13 110.2(3) . . ?
C17 C15 C11 110.4(3) . . ?
C17 C15 C16 108.6(4) . . ?
C11 C15 C16 113.2(4) . . ?
C19 C18 C23 121.4(3) . . ?
C19 C18 N2 121.2(3) . . ?
C23 C18 N2 117.3(3) . . ?
C20 C19 C18 118.0(3) . . ?
C20 C19 C24 118.6(3) . . ?
C18 C19 C24 123.4(3) . . ?
C21 C20 C19 121.2(4) . . ?
C22 C21 C20 119.9(4) . . ?
C21 C22 C23 121.2(4) . . ?
C22 C23 C18 117.7(4) . . ?
C22 C23 C27 119.6(3) . . ?
C18 C23 C27 122.7(3) . . ?
C19 C24 C25 114.1(3) . . ?
C19 C24 C26 109.1(3) . . ?
C25 C24 C26 109.6(4) . . ?
C28 C27 C23 110.3(4) . . ?
C28 C27 C29 110.9(5) . . ?
C23 C27 C29 112.1(4) . . ?
O1 C30 W1 178.0(5) . . ?
O2 C31 W1 177.4(4) . . ?
O3 C32 W1 177.8(4) . . ?
O4 C33 W1 179.1(5) . . ?
O5 C34 W1 176.2(4) . . ?
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
W1 C32 2.001(5) . ?
W1 C33 2.027(5) . ?
W1 C30 2.031(5) . ?
W1 C34 2.035(5) . ?
W1 C31 2.041(5) . ?
W1 Ge1 2.5564(6) . ?
Ge1 N1 1.961(3) . ?
Ge1 N2 1.978(3) . ?
Ge1 Cl1 2.2091(10) . ?
O1 C30 1.142(6) . ?
N1 C1 1.352(4) . ?
N1 C6 1.431(5) . ?
C1 N2 1.340(4) . ?
C1 C2 1.533(5) . ?
O2 C31 1.134(5) . ?
N2 C18 1.443(4) . ?
C2 C3A 1.460(10) . ?
C2 C5 1.488(8) . ?
C2 C5A 1.521(11) . ?
C2 C4 1.536(8) . ?
C2 C3 1.601(8) . ?
C2 C4A 1.653(11) . ?
O3 C32 1.148(5) . ?
O4 C33 1.156(6) . ?
O5 C34 1.151(5) . ?
C6 C7 1.408(5) . ?
C6 C11 1.418(5) . ?
C7 C8 1.384(6) . ?
C7 C12 1.523(5) . ?
C8 C9 1.388(6) . ?
C9 C10 1.384(6) . ?
C10 C11 1.392(5) . ?
C11 C15 1.530(5) . ?
C12 C14 1.526(6) . ?
C12 C13 1.553(5) . ?
C15 C17 1.507(6) . ?
C15 C16 1.531(5) . ?
C18 C19 1.396(5) . ?
C18 C23 1.411(5) . ?
C19 C20 1.391(5) . ?
C19 C24 1.521(5) . ?
C20 C21 1.386(6) . ?
C21 C22 1.377(6) . ?
C22 C23 1.394(6) . ?
C23 C27 1.521(6) . ?
C24 C25 1.530(6) . ?
C24 C26 1.531(5) . ?
C27 C28 1.518(7) . ?
C27 C29 1.531(7) . ?
