#------------------------------------------------------------------------------
#$Date: 2019-11-23 15:57:10 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233911 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/93/4349383.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_4349383
loop_
_publ_author_name
'Weßing, Jana'
'Göbel, Christoph'
'Weber, Birgit'
'Gemel, Christian'
'Fischer, Roland A.'
_publ_section_title
;
 Diverse Reactivity of ECp* (E = Al, Ga) toward Low-Coordinate Transition
 Metal Amides [TM(N(SiMe₃)₂)₂] (TM = Fe,
 Co, Zn): Insertion, Cp* Transfer, and Orthometalation.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3517
_journal_page_last               3525
_journal_paper_doi               10.1021/acs.inorgchem.6b03127
_journal_volume                  56
_journal_year                    2017
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C32 H66 Al2 N2 Si4 Zn'
_chemical_formula_sum            'C32 H66 Al2 N2 Si4 Zn'
_chemical_formula_weight         710.58
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                93.962(5)
_cell_angle_beta                 106.393(5)
_cell_angle_gamma                112.654(5)
_cell_formula_units_Z            1
_cell_length_a                   8.5944(5)
_cell_length_b                   9.6962(5)
_cell_length_c                   14.0679(9)
_cell_measurement_reflns_used    3497
_cell_measurement_temperature    113
_cell_measurement_theta_max      75.8680
_cell_measurement_theta_min      5.0250
_cell_volume                     1016.75(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 10.4372
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'SuperNova, Agilent Technologies'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7520
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        67.68
_diffrn_reflns_theta_max         76.35
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    2.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         4172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[Σ²(FO²)+(0.0479P)²+0.2727P] WHERE P=(FO²+2FC²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                3490
_reflns_number_total             4172
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic6b03127_si_001.cif
_cod_data_source_block           om1214
_cod_database_code               4349383
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn Uani 0.00000 0.00000 0.50000 1.000 0.0193(1) d SP
Si1 Si Uani -0.12952(7) -0.16865(6) 0.14795(4) 1.000 0.0199(2) d .
Si2 Si Uani -0.48316(7) -0.23813(6) 0.18435(4) 1.000 0.0202(2) d .
Al1 Al Uani -0.13577(8) 0.02314(7) 0.32726(4) 1.000 0.0174(2) d .
N1 N Uani -0.2565(2) -0.12953(19) 0.21248(12) 1.000 0.0184(5) d .
C1 C Uani -0.1299(3) -0.3625(3) 0.14898(19) 1.000 0.0318(7) d .
C2 C Uani -0.2044(3) -0.1524(3) 0.01216(16) 1.000 0.0285(6) d .
C3 C Uani 0.1109(3) -0.0306(3) 0.21102(17) 1.000 0.0275(6) d .
C4 C Uani -0.6223(3) -0.1976(3) 0.07060(18) 1.000 0.0315(7) d .
C5 C Uani -0.5504(3) -0.4487(3) 0.1557(2) 1.000 0.0332(7) d .
C6 C Uani -0.5484(3) -0.2017(3) 0.29669(17) 1.000 0.0277(7) d .
C7 C Uani -0.2056(3) 0.2199(2) 0.32749(16) 1.000 0.0217(6) d .
C8 C Uani -0.1384(3) 0.2636(2) 0.43455(17) 1.000 0.0242(6) d .
C9 C Uani 0.0485(3) 0.3200(2) 0.46759(16) 1.000 0.0227(6) d .
C10 C Uani 0.1027(3) 0.3127(2) 0.38210(16) 1.000 0.0214(6) d .
C11 C Uani -0.0522(3) 0.2520(2) 0.29430(15) 1.000 0.0194(5) d .
C12 C Uani -0.3867(3) 0.1984(3) 0.2591(2) 1.000 0.0327(7) d .
C13 C Uani -0.2482(4) 0.2500(3) 0.5029(2) 1.000 0.0364(8) d .
C14 C Uani 0.1722(3) 0.3803(3) 0.57568(17) 1.000 0.0327(7) d .
C15 C Uani 0.2922(3) 0.3639(3) 0.38385(19) 1.000 0.0302(7) d .
C16 C Uani -0.0577(3) 0.2633(3) 0.18680(16) 1.000 0.0289(7) d .
H1A H Uiso -0.25050 -0.44110 0.11160 1.000 0.0480 c RU
H1B H Uiso -0.09370 -0.37610 0.21900 1.000 0.0480 c RU
H1C H Uiso -0.04580 -0.37130 0.11690 1.000 0.0480 c RU
H2A H Uiso -0.12600 -0.17020 -0.02120 1.000 0.0430 c RU
H2B H Uiso -0.19840 -0.04990 0.00860 1.000 0.0430 c RU
H2C H Uiso -0.32780 -0.22840 -0.02190 1.000 0.0430 c RU
H3A H Uiso 0.18430 -0.05220 0.17530 1.000 0.0410 c RU
H3B H Uiso 0.15140 -0.04110 0.28150 1.000 0.0410 c RU
H3C H Uiso 0.12260 0.07370 0.20920 1.000 0.0410 c RU
H4A H Uiso -0.59780 -0.22830 0.01060 1.000 0.0470 c RU
H4B H Uiso -0.59250 -0.08820 0.08060 1.000 0.0470 c RU
H4C H Uiso -0.74940 -0.25510 0.06120 1.000 0.0470 c RU
H5A H Uiso -0.67650 -0.50360 0.14930 1.000 0.0500 c RU
H5B H Uiso -0.47620 -0.47650 0.21070 1.000 0.0500 c RU
H5C H Uiso -0.53360 -0.47620 0.09220 1.000 0.0500 c RU
H6A H Uiso -0.51290 -0.09210 0.31630 1.000 0.0420 c RU
H6B H Uiso -0.48820 -0.23710 0.35320 1.000 0.0420 c RU
H6C H Uiso -0.67830 -0.25670 0.27940 1.000 0.0420 c RU
H12A H Uiso -0.38270 0.29740 0.24590 1.000 0.0490 c RU
H12B H Uiso -0.47610 0.15350 0.29170 1.000 0.0490 c RU
H12C H Uiso -0.41910 0.13020 0.19500 1.000 0.0490 c RU
H13A H Uiso -0.37550 0.20560 0.46210 1.000 0.0550 c RU
H13B H Uiso -0.21440 0.35140 0.54130 1.000 0.0550 c RU
H13C H Uiso -0.22620 0.18410 0.54990 1.000 0.0550 c RU
H14A H Uiso 0.29590 0.40890 0.57800 1.000 0.0490 c RU
H14B H Uiso 0.14000 0.30120 0.61540 1.000 0.0490 c RU
H14C H Uiso 0.16130 0.47000 0.60400 1.000 0.0490 c RU
H15A H Uiso 0.29250 0.32770 0.31710 1.000 0.0450 c RU
H15B H Uiso 0.35500 0.32170 0.43460 1.000 0.0450 c RU
H15C H Uiso 0.35300 0.47550 0.40090 1.000 0.0450 c RU
H16A H Uiso -0.15390 0.17050 0.14040 1.000 0.0430 c RU
H16B H Uiso 0.05710 0.27470 0.18040 1.000 0.0430 c RU
H16C H Uiso -0.07960 0.35200 0.16990 1.000 0.0430 c RU
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'
Al Al 0.2130 0.2455 ' 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'
Si Si 0.2541 0.3302 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 ' 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_3
_geom_angle_publ_flag
Al1 Zn1 Al1 180.00 2_556 yes
N1 Si1 C1 114.80(11) . yes
N1 Si1 C2 111.64(11) . yes
N1 Si1 C3 108.78(10) . yes
C1 Si1 C2 107.08(12) . yes
C1 Si1 C3 104.89(12) . yes
C2 Si1 C3 109.35(12) . yes
N1 Si2 C4 112.50(11) . yes
N1 Si2 C5 113.62(11) . yes
N1 Si2 C6 109.17(10) . yes
C4 Si2 C5 105.37(12) . yes
C4 Si2 C6 109.90(12) . yes
C5 Si2 C6 106.03(12) . yes
Zn1 Al1 N1 127.59(6) . yes
Zn1 Al1 C7 111.01(6) . yes
Zn1 Al1 C11 117.21(6) . yes
N1 Al1 C7 116.87(9) . yes
N1 Al1 C11 113.28(8) . yes
C7 Al1 C11 38.58(10) . yes
Si1 N1 Si2 123.81(10) . yes
Si1 N1 Al1 117.23(11) . yes
Si2 N1 Al1 118.53(10) . yes
Al1 C7 C8 93.59(14) . yes
Al1 C7 C11 69.65(12) . yes
Al1 C7 C12 118.62(15) . yes
C8 C7 C11 106.9(2) . no
C8 C7 C12 126.4(2) . no
C11 C7 C12 123.6(2) . no
C7 C8 C9 109.0(2) . no
C7 C8 C13 126.2(2) . no
C9 C8 C13 124.9(2) . no
C8 C9 C10 108.5(2) . no
C8 C9 C14 126.1(2) . no
C10 C9 C14 125.4(2) . no
C9 C10 C11 108.4(2) . no
C9 C10 C15 125.8(2) . no
C11 C10 C15 125.9(2) . no
Al1 C11 C7 71.77(11) . yes
Al1 C11 C10 92.63(12) . yes
Al1 C11 C16 116.19(15) . yes
C7 C11 C10 107.29(19) . no
C7 C11 C16 123.8(2) . no
C10 C11 C16 126.5(2) . no
Si1 C1 H1A 109.00 . no
Si1 C1 H1B 109.00 . no
Si1 C1 H1C 109.00 . no
H1A C1 H1B 109.00 . no
H1A C1 H1C 109.00 . no
H1B C1 H1C 110.00 . no
Si1 C2 H2A 109.00 . no
Si1 C2 H2B 109.00 . no
Si1 C2 H2C 109.00 . no
H2A C2 H2B 109.00 . no
H2A C2 H2C 110.00 . no
H2B C2 H2C 109.00 . no
Si1 C3 H3A 109.00 . no
Si1 C3 H3B 109.00 . no
Si1 C3 H3C 109.00 . no
H3A C3 H3B 110.00 . no
H3A C3 H3C 109.00 . no
H3B C3 H3C 109.00 . no
Si2 C4 H4A 110.00 . no
Si2 C4 H4B 109.00 . no
Si2 C4 H4C 109.00 . no
H4A C4 H4B 109.00 . no
H4A C4 H4C 109.00 . no
H4B C4 H4C 109.00 . no
Si2 C5 H5A 110.00 . no
Si2 C5 H5B 109.00 . no
Si2 C5 H5C 109.00 . no
H5A C5 H5B 109.00 . no
H5A C5 H5C 109.00 . no
H5B C5 H5C 109.00 . no
Si2 C6 H6A 109.00 . no
Si2 C6 H6B 110.00 . no
Si2 C6 H6C 110.00 . no
H6A C6 H6B 109.00 . no
H6A C6 H6C 109.00 . no
H6B C6 H6C 109.00 . no
C7 C12 H12A 109.00 . no
C7 C12 H12B 110.00 . no
C7 C12 H12C 109.00 . no
H12A C12 H12B 110.00 . no
H12A C12 H12C 109.00 . no
H12B C12 H12C 109.00 . no
C8 C13 H13A 110.00 . no
C8 C13 H13B 109.00 . no
C8 C13 H13C 109.00 . no
H13A C13 H13B 109.00 . no
H13A C13 H13C 109.00 . no
H13B C13 H13C 109.00 . no
C9 C14 H14A 109.00 . no
C9 C14 H14B 109.00 . no
C9 C14 H14C 110.00 . no
H14A C14 H14B 109.00 . no
H14A C14 H14C 109.00 . no
H14B C14 H14C 109.00 . no
C10 C15 H15A 109.00 . no
C10 C15 H15B 110.00 . no
C10 C15 H15C 110.00 . no
H15A C15 H15B 109.00 . no
H15A C15 H15C 109.00 . no
H15B C15 H15C 109.00 . no
C11 C16 H16A 110.00 . no
C11 C16 H16B 109.00 . no
C11 C16 H16C 109.00 . no
H16A C16 H16B 109.00 . no
H16A C16 H16C 110.00 . no
H16B C16 H16C 109.00 . no
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
Zn1 Al1 2.4482(6) . yes
Zn1 Al1 2.4482(6) 2_556 yes
Si1 N1 1.729(2) . yes
Si1 C1 1.879(3) . yes
Si1 C2 1.875(2) . yes
Si1 C3 1.876(3) . yes
Si2 N1 1.728(2) . yes
Si2 C4 1.875(3) . yes
Si2 C5 1.874(3) . yes
Si2 C6 1.874(3) . yes
Al1 N1 1.8483(17) . yes
Al1 C7 2.210(2) . yes
Al1 C11 2.181(2) . yes
C7 C8 1.419(3) . no
C7 C11 1.451(4) . no
C7 C12 1.506(4) . no
C8 C9 1.401(4) . no
C8 C13 1.505(4) . no
C9 C10 1.414(3) . no
C9 C14 1.507(3) . no
C10 C11 1.419(3) . no
C10 C15 1.501(4) . no
C11 C16 1.513(3) . no
C1 H1A 0.9800 . no
C1 H1B 0.9800 . no
C1 H1C 0.9800 . no
C2 H2A 0.9800 . no
C2 H2B 0.9800 . no
C2 H2C 0.9800 . no
C3 H3A 0.9800 . no
C3 H3B 0.9800 . no
C3 H3C 0.9800 . no
C4 H4A 0.9800 . no
C4 H4B 0.9800 . no
C4 H4C 0.9800 . no
C5 H5A 0.9800 . no
C5 H5B 0.9800 . no
C5 H5C 0.9800 . no
C6 H6A 0.9800 . no
C6 H6B 0.9800 . no
C6 H6C 0.9800 . no
C12 H12A 0.9800 . no
C12 H12B 0.9800 . no
C12 H12C 0.9800 . no
C13 H13A 0.9800 . no
C13 H13B 0.9800 . no
C13 H13C 0.9800 . no
C14 H14A 0.9800 . no
C14 H14B 0.9800 . no
C14 H14C 0.9800 . no
C15 H15A 0.9800 . no
C15 H15B 0.9800 . no
C15 H15C 0.9800 . no
C16 H16A 0.9800 . no
C16 H16B 0.9800 . no
C16 H16C 0.9800 . no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
C1 Si1 N1 Si2 -58.40(15) no
C1 Si1 N1 Al1 113.93(13) no
C2 Si1 N1 Si2 63.70(15) no
C2 Si1 N1 Al1 -123.97(12) no
C3 Si1 N1 Si2 -175.54(12) no
C3 Si1 N1 Al1 -3.21(14) no
C4 Si2 N1 Si1 -77.98(15) no
C4 Si2 N1 Al1 109.78(13) no
C5 Si2 N1 Si1 41.64(16) no
C5 Si2 N1 Al1 -130.60(12) no
C6 Si2 N1 Si1 159.74(13) no
C6 Si2 N1 Al1 -12.50(15) no
Zn1 Al1 N1 Si1 -86.18(11) no
C7 Al1 N1 Si1 120.02(11) no
C11 Al1 N1 Si1 77.42(13) no
Zn1 Al1 N1 Si2 86.57(12) no
C7 Al1 N1 Si2 -67.23(13) no
C11 Al1 N1 Si2 -109.83(12) no
Zn1 Al1 C7 C8 1.03(16) no
N1 Al1 C7 C8 159.01(14) no
C11 Al1 C7 C8 -106.7(2) no
Zn1 Al1 C7 C11 107.69(11) no
N1 Al1 C7 C11 -94.32(14) no
Zn1 Al1 C7 C12 -134.30(17) no
N1 Al1 C7 C12 23.7(2) no
C11 Al1 C7 C12 118.0(2) no
N1 Al1 C11 C10 -148.21(15) no
C7 Al1 C11 C10 107.34(19) no
Zn1 Al1 C11 C16 150.51(17) no
N1 Al1 C11 C16 -14.9(2) no
C7 Al1 C11 C16 -119.4(2) no
Zn1 Al1 C11 C10 17.22(18) no
Zn1 Al1 C11 C7 -90.12(12) no
N1 Al1 C11 C7 104.45(13) no
C12 C7 C8 C13 20.5(3) no
C8 C7 C11 C10 0.5(2) no
C8 C7 C11 C16 -162.7(2) no
C12 C7 C11 Al1 -111.5(2) no
C12 C7 C11 C10 161.4(2) no
Al1 C7 C11 C10 -87.03(14) no
Al1 C7 C11 C16 109.8(2) no
C8 C7 C11 Al1 87.55(14) no
Al1 C7 C8 C9 69.56(16) no
Al1 C7 C8 C13 -109.5(2) no
C11 C7 C8 C9 -0.3(2) no
C11 C7 C8 C13 -179.3(2) no
C12 C7 C8 C9 -160.5(2) no
C12 C7 C11 C16 -1.7(3) no
C7 C8 C9 C10 -0.1(2) no
C7 C8 C9 C14 179.2(2) no
C13 C8 C9 C10 179.0(2) no
C13 C8 C9 C14 -1.7(3) no
C8 C9 C10 C11 0.4(2) no
C8 C9 C10 C15 179.1(2) no
C14 C9 C10 C15 -0.2(3) no
C14 C9 C10 C11 -178.9(2) no
C9 C10 C11 C7 -0.6(2) no
C9 C10 C11 C16 162.0(2) no
C9 C10 C11 Al1 -72.31(16) no
C15 C10 C11 C7 -179.3(2) no
C15 C10 C11 C16 -16.7(4) no
C15 C10 C11 Al1 109.0(2) no
