#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:01:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180000 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/94/7029482.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_7029482
loop_
_publ_author_name
'Tan, Gengwen'
'Wang, Wenyuan'
'Blom, Burgert'
'Driess, Matthias'
_publ_section_title
;
 Mechanistic studies of CO2 reduction to methanol mediated by an
 N-heterocyclic germylene hydride.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6006
_journal_page_last               6011
_journal_paper_doi               10.1039/c3dt53321b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C59 H84 Al Ge N4 O2'
_chemical_formula_weight         980.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.2710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.8625(3)
_cell_length_b                   15.1844(2)
_cell_length_c                   14.7693(2)
_cell_measurement_reflns_used    6570
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4740
_cell_measurement_theta_min      4.4720
_cell_volume                     5560.25(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10763
_diffrn_reflns_theta_full        73.62
_diffrn_reflns_theta_max         73.62
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_T_max  0.9092
_exptl_absorpt_correction_T_min  0.8666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.00014(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5448
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0437
_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)+(0.0718P)²+6.8210P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                5030
_reflns_number_total             5448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53321b.txt
_cod_data_source_block           c2c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7029482
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Al1 Al 0.32457(5) 0.28268(9) 1.07708(8) 0.0222(3) Uani 0.50 1 d PD
H1 H 0.2824(17) 0.333(3) 1.098(3) 0.027 Uiso 1 1 d D
Ge1 Ge 0.172831(18) 0.24889(4) 0.95382(4) 0.02525(15) Uani 0.50 1 d P
N1 N 0.14301(5) 0.29210(9) 0.83088(9) 0.0218(3) Uani 1 1 d .
N2 N 0.10957(5) 0.16432(8) 0.95574(9) 0.0200(3) Uani 1 1 d .
C1 C 0.08739(9) 0.29663(15) 0.68543(12) 0.0414(5) Uani 1 1 d .
H1A H 0.0841 0.3606 0.6917 0.062 Uiso 1 1 calc R
H1B H 0.0527 0.2721 0.6618 0.062 Uiso 1 1 calc R
H1C H 0.1149 0.2832 0.6433 0.062 Uiso 1 1 calc R
C2 C 0.10353(7) 0.25646(11) 0.77709(11) 0.0265(4) Uani 1 1 d .
C3 C 0.07404(6) 0.18287(12) 0.80163(11) 0.0270(4) Uani 1 1 d .
H3A H 0.0519 0.1557 0.7544 0.032 Uiso 1 1 calc R
C4 C 0.07347(6) 0.14476(10) 0.88777(11) 0.0223(3) Uani 1 1 d .
C5 C 0.02766(7) 0.08243(12) 0.90309(12) 0.0297(4) Uani 1 1 d .
H5A H 0.0418 0.0306 0.9365 0.045 Uiso 1 1 calc R
H5B H 0.0103 0.0640 0.8444 0.045 Uiso 1 1 calc R
H5C H 0.0012 0.1123 0.9383 0.045 Uiso 1 1 calc R
C6 C 0.16699(6) 0.37380(10) 0.80241(10) 0.0233(3) Uani 1 1 d .
C7 C 0.14798(7) 0.45387(11) 0.83580(12) 0.0275(4) Uani 1 1 d .
C8 C 0.16796(8) 0.53159(11) 0.80158(13) 0.0335(4) Uani 1 1 d .
H8A H 0.1548 0.5863 0.8219 0.040 Uiso 1 1 calc R
C9 C 0.20649(8) 0.53121(12) 0.73871(13) 0.0349(4) Uani 1 1 d .
H9A H 0.2186 0.5850 0.7145 0.042 Uiso 1 1 calc R
C10 C 0.22718(8) 0.45206(12) 0.71139(12) 0.0319(4) Uani 1 1 d .
H10A H 0.2549 0.4522 0.6705 0.038 Uiso 1 1 calc R
C11 C 0.20827(7) 0.37160(11) 0.74251(11) 0.0262(3) Uani 1 1 d .
C12 C 0.23406(8) 0.28672(11) 0.71288(12) 0.0313(4) Uani 1 1 d .
H12A H 0.2140 0.2362 0.7377 0.038 Uiso 1 1 calc R
C13 C 0.29245(9) 0.28195(13) 0.75201(15) 0.0406(5) Uani 1 1 d .
H13A H 0.2935 0.2809 0.8185 0.061 Uiso 1 1 calc R
H13B H 0.3122 0.3336 0.7324 0.061 Uiso 1 1 calc R
H13C H 0.3093 0.2283 0.7304 0.061 Uiso 1 1 calc R
C14 C 0.23168(10) 0.27755(15) 0.60917(13) 0.0459(5) Uani 1 1 d .
H14A H 0.1943 0.2847 0.5840 0.069 Uiso 1 1 calc R
H14B H 0.2449 0.2192 0.5932 0.069 Uiso 1 1 calc R
H14C H 0.2543 0.3230 0.5841 0.069 Uiso 1 1 calc R
C15 C 0.10654(8) 0.45637(12) 0.90669(14) 0.0350(4) Uani 1 1 d .
H15A H 0.1086 0.3986 0.9393 0.042 Uiso 1 1 calc R
C16 C 0.11848(9) 0.52821(16) 0.97755(16) 0.0488(5) Uani 1 1 d .
H16A H 0.1554 0.5213 1.0047 0.073 Uiso 1 1 calc R
H16B H 0.0931 0.5233 1.0250 0.073 Uiso 1 1 calc R
H16C H 0.1146 0.5861 0.9485 0.073 Uiso 1 1 calc R
C17 C 0.04947(9) 0.4654(2) 0.8635(2) 0.0643(7) Uani 1 1 d .
H17A H 0.0412 0.4153 0.8230 0.096 Uiso 1 1 calc R
H17B H 0.0464 0.5202 0.8284 0.096 Uiso 1 1 calc R
H17C H 0.0240 0.4666 0.9110 0.096 Uiso 1 1 calc R
C18 C 0.10161(6) 0.13081(10) 1.04555(10) 0.0220(3) Uani 1 1 d .
C19 C 0.12264(6) 0.04835(11) 1.07228(11) 0.0254(3) Uani 1 1 d .
C20 C 0.11382(8) 0.01821(13) 1.15936(12) 0.0341(4) Uani 1 1 d .
H20A H 0.1274 -0.0378 1.1787 0.041 Uiso 1 1 calc R
C21 C 0.08569(8) 0.06864(14) 1.21775(13) 0.0386(4) Uani 1 1 d .
H21A H 0.0797 0.0471 1.2766 0.046 Uiso 1 1 calc R
C22 C 0.06626(8) 0.15031(13) 1.19063(12) 0.0353(4) Uani 1 1 d .
H22A H 0.0474 0.1847 1.2316 0.042 Uiso 1 1 calc R
C23 C 0.07367(6) 0.18351(12) 1.10461(12) 0.0277(4) Uani 1 1 d .
C24 C 0.05171(7) 0.27372(12) 1.07707(13) 0.0335(4) Uani 1 1 d .
H24A H 0.0637 0.2868 1.0154 0.040 Uiso 1 1 calc R
C25 C -0.01011(9) 0.27505(17) 1.06955(18) 0.0518(6) Uani 1 1 d .
H25A H -0.0229 0.3318 1.0447 0.078 Uiso 1 1 calc R
H25B H -0.0233 0.2667 1.1299 0.078 Uiso 1 1 calc R
H25C H -0.0237 0.2275 1.0292 0.078 Uiso 1 1 calc R
C26 C 0.07424(10) 0.34522(15) 1.14032(19) 0.0537(6) Uani 1 1 d .
H26A H 0.1137 0.3445 1.1422 0.081 Uiso 1 1 calc R
H26B H 0.0627 0.3349 1.2014 0.081 Uiso 1 1 calc R
H26C H 0.0609 0.4027 1.1183 0.081 Uiso 1 1 calc R
C27 C 0.15483(7) -0.00834(11) 1.01124(12) 0.0300(4) Uani 1 1 d .
H27A H 0.1580 0.0239 0.9528 0.036 Uiso 1 1 calc R
C28 C 0.12781(10) -0.09688(14) 0.98977(17) 0.0494(5) Uani 1 1 d .
H28A H 0.0913 -0.0871 0.9617 0.074 Uiso 1 1 calc R
H28B H 0.1258 -0.1306 1.0460 0.074 Uiso 1 1 calc R
H28C H 0.1489 -0.1299 0.9478 0.074 Uiso 1 1 calc R
C29 C 0.21128(10) -0.0238(2) 1.0550(2) 0.0707(9) Uani 1 1 d .
H29A H 0.2291 0.0330 1.0672 0.106 Uiso 1 1 calc R
H29B H 0.2321 -0.0585 1.0139 0.106 Uiso 1 1 calc R
H29C H 0.2090 -0.0559 1.1122 0.106 Uiso 1 1 calc R
C50 C 0.26549(13) 0.1504(2) 0.9748(2) 0.0251(6) Uani 0.50 1 d P
O1 O 0.22286(17) 0.1738(3) 0.9124(3) 0.0249(6) Uani 0.50 1 d P
O2A O 0.30754(9) 0.21102(17) 0.97922(15) 0.0289(5) Uani 0.50 1 d P
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'
Al Al 0.2130 0.2455 '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'
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
Ge1 Al1 O1 123.4(2) 7_557 7_557
Ge1 Al1 O2A 20.67(12) 7_557 .
O1 Al1 O2A 103.03(18) 7_557 .
Ge1 Al1 N1 90.14(14) 7_557 7_557
O1 Al1 N1 121.9(2) 7_557 7_557
O2A Al1 N1 105.64(11) . 7_557
Ge1 Al1 N2 90.03(14) 7_557 7_557
O1 Al1 N2 125.7(2) 7_557 7_557
O2A Al1 N2 101.60(10) . 7_557
N1 Al1 N2 96.11(8) 7_557 7_557
Al1 Ge1 O2A 148.29(19) 7_557 7_557
Al1 Ge1 O1 38.77(16) 7_557 .
O2A Ge1 O1 109.80(16) 7_557 .
Al1 Ge1 N1 70.53(13) 7_557 .
O2A Ge1 N1 131.22(13) 7_557 .
O1 Ge1 N1 96.62(14) . .
Al1 Ge1 N2 70.78(13) 7_557 .
O2A Ge1 N2 124.22(12) 7_557 .
O1 Ge1 N2 99.05(14) . .
N1 Ge1 N2 89.14(6) . .
Al1 Ge1 C50 132.65(15) 7_557 7_557
O2A Ge1 C50 27.67(14) 7_557 7_557
O1 Ge1 C50 96.78(14) . 7_557
N1 Ge1 C50 111.98(9) . 7_557
N2 Ge1 C50 151.86(9) . 7_557
C2 N1 C6 118.36(13) . .
C2 N1 Al1 115.98(12) . 7_557
C6 N1 Al1 123.72(11) . 7_557
C2 N1 Ge1 127.58(11) . .
C6 N1 Ge1 114.00(10) . .
Al1 N1 Ge1 19.33(4) 7_557 .
C4 N2 C18 118.86(13) . .
C4 N2 Al1 116.35(11) . 7_557
C18 N2 Al1 123.79(10) . 7_557
C4 N2 Ge1 127.61(11) . .
C18 N2 Ge1 113.17(9) . .
Al1 N2 Ge1 19.20(4) 7_557 .
N1 C2 C3 123.20(15) . .
N1 C2 C1 120.35(15) . .
C3 C2 C1 116.43(15) . .
C4 C3 C2 127.38(15) . .
N2 C4 C3 122.85(14) . .
N2 C4 C5 120.06(14) . .
C3 C4 C5 117.02(14) . .
C11 C6 C7 121.45(15) . .
C11 C6 N1 119.81(14) . .
C7 C6 N1 118.74(14) . .
C8 C7 C6 117.88(16) . .
C8 C7 C15 120.47(16) . .
C6 C7 C15 121.64(15) . .
C9 C8 C7 121.66(17) . .
C10 C9 C8 119.48(16) . .
C9 C10 C11 121.53(17) . .
C10 C11 C6 117.74(16) . .
C10 C11 C12 119.16(15) . .
C6 C11 C12 123.08(14) . .
C11 C12 C13 109.99(15) . .
C11 C12 C14 112.27(16) . .
C13 C12 C14 109.82(16) . .
C17 C15 C7 111.84(18) . .
C17 C15 C16 110.60(17) . .
C7 C15 C16 112.48(16) . .
C19 C18 C23 121.67(15) . .
C19 C18 N2 119.88(14) . .
C23 C18 N2 118.44(14) . .
C20 C19 C18 118.08(16) . .
C20 C19 C27 119.13(16) . .
C18 C19 C27 122.78(15) . .
C21 C20 C19 120.94(18) . .
C22 C21 C20 119.97(17) . .
C21 C22 C23 121.56(17) . .
C22 C23 C18 117.75(17) . .
C22 C23 C24 120.11(16) . .
C18 C23 C24 122.14(15) . .
C26 C24 C23 111.89(17) . .
C26 C24 C25 111.01(17) . .
C23 C24 C25 111.70(17) . .
C19 C27 C29 110.27(16) . .
C19 C27 C28 112.32(16) . .
C29 C27 C28 109.31(19) . .
O2A C50 O1 113.1(3) . .
O2A C50 Ge1 24.27(12) . 7_557
O1 C50 Ge1 124.5(3) . 7_557
Al1 O1 C50 131.6(4) 7_557 .
Al1 O1 Ge1 17.78(9) 7_557 .
C50 O1 Ge1 116.1(3) . .
Ge1 O2A C50 128.1(2) 7_557 .
Ge1 O2A Al1 11.05(7) 7_557 .
C50 O2A Al1 123.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 Ge1 0.6683(11) 7_557
Al1 O1 1.371(5) 7_557
Al1 O2A 1.833(3) .
Al1 N1 1.9037(17) 7_557
Al1 N2 1.9191(17) 7_557
Ge1 Al1 0.6683(11) 7_557
Ge1 O2A 1.231(2) 7_557
Ge1 O1 1.826(5) .
Ge1 N1 2.0191(14) .
Ge1 N2 2.0324(14) .
Ge1 C50 2.358(3) 7_557
N1 C2 1.331(2) .
N1 C6 1.452(2) .
N1 Al1 1.9037(17) 7_557
N2 C4 1.329(2) .
N2 C18 1.4479(19) .
N2 Al1 1.9191(17) 7_557
C1 C2 1.512(2) .
C2 C3 1.399(2) .
C3 C4 1.399(2) .
C4 C5 1.511(2) .
C6 C11 1.405(2) .
C6 C7 1.407(2) .
C7 C8 1.390(2) .
C7 C15 1.523(3) .
C8 C9 1.383(3) .
C9 C10 1.380(3) .
C10 C11 1.399(2) .
C11 C12 1.518(2) .
C12 C13 1.524(3) .
C12 C14 1.535(2) .
C15 C17 1.518(3) .
C15 C16 1.525(3) .
C18 C19 1.402(2) .
C18 C23 1.405(2) .
C19 C20 1.398(2) .
C19 C27 1.517(2) .
C20 C21 1.382(3) .
C21 C22 1.379(3) .
C22 C23 1.392(2) .
C23 C24 1.519(3) .
C24 C26 1.512(3) .
C24 C25 1.533(3) .
C27 C29 1.519(3) .
C27 C28 1.526(3) .
C50 O2A 1.391(4) .
C50 O1 1.398(5) .
C50 Ge1 2.358(3) 7_557
O1 Al1 1.371(5) 7_557
O2A Ge1 1.231(2) 7_557
