#------------------------------------------------------------------------------
#$Date: 2019-01-26 01:02:54 +0200 (Sat, 26 Jan 2019) $
#$Revision: 213328 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/29/7122901.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_7122901
loop_
_publ_author_name
'Roesky, Herbert W.'
'Li, Jiancheng'
'Mingdong, Zhong'
'Keil, Helena'
'Zhu, Hongping'
'Herbst-Irmer, Regine'
'Stalke, Dietmar'
'Koley, Debasis'
'De, Sriman'
_publ_section_title
;
 (PhC(NtBu)2Al)2(SiH2)4 Six-Membered Heterocycle: Comparable in Structure
 to Cyclohexane
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC10124H
_journal_year                    2019
_chemical_formula_moiety         'C48 H74 Al2 N4 Si2'
_chemical_formula_sum            'C48 H74 Al2 N4 Si2'
_chemical_formula_weight         817.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-10-24 deposited with the CCDC.
2019-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                103.40(2)
_cell_angle_beta                 97.39(2)
_cell_angle_gamma                114.85(3)
_cell_formula_units_Z            1
_cell_length_a                   10.039(2)
_cell_length_b                   10.144(2)
_cell_length_c                   13.835(3)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.207
_cell_measurement_theta_min      2.196
_cell_volume                     1202.2(6)
_computing_cell_refinement       'SAINT V8.38A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.38A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46064
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.548
_diffrn_reflns_theta_min         1.825
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.7215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4929
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0380P)²+0.6554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4013
_reflns_number_total             4929
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc10124h2.cif
_cod_data_source_block           sad_a
_cod_original_cell_volume        1202.2(5)
_cod_database_code               7122901
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.988
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
H2X H 0.834(2) 0.399(2) 0.4058(15) 0.040(5) Uiso 1 1 d D . . . .
H2Y H 0.876(2) 0.6226(19) 0.3856(15) 0.039(5) Uiso 1 1 d D . . . .
C3 C 1.03956(18) 0.66197(19) 0.82245(13) 0.0234(4) Uani 1 1 d . . . . .
H3 H 1.079395 0.634759 0.766788 0.028 Uiso 1 1 calc R U . . .
C4 C 1.11908(19) 0.6994(2) 0.92276(14) 0.0310(4) Uani 1 1 d . . . . .
H4 H 1.213313 0.697263 0.935612 0.037 Uiso 1 1 calc R U . . .
C7 C 0.84624(18) 0.7078(2) 0.88594(12) 0.0235(4) Uani 1 1 d . . . . .
H7 H 0.752661 0.711320 0.873674 0.028 Uiso 1 1 calc R U . . .
C6 C 0.9273(2) 0.7457(2) 0.98536(13) 0.0304(4) Uani 1 1 d . . . . .
H6 H 0.889679 0.776265 1.041416 0.037 Uiso 1 1 calc R U . . .
C5 C 1.0624(2) 0.7395(2) 1.00386(13) 0.0308(4) Uani 1 1 d . . . . .
H5 H 1.116239 0.762865 1.072335 0.037 Uiso 1 1 calc R U . . .
C8 C 0.92028(17) 0.87069(17) 0.66262(12) 0.0191(3) Uani 1 1 d . . . . .
C9 C 0.85917(19) 0.91804(18) 0.57726(13) 0.0249(4) Uani 1 1 d . . . . .
H9A H 0.854463 0.854290 0.510474 0.037 Uiso 1 1 calc R U . . .
H9B H 0.926596 1.025891 0.586777 0.037 Uiso 1 1 calc R U . . .
H9C H 0.757172 0.904359 0.579692 0.037 Uiso 1 1 calc R U . . .
C11 C 0.9232(2) 0.96960(18) 0.76542(13) 0.0265(4) Uani 1 1 d . . . . .
H11A H 0.978112 1.078003 0.770814 0.040 Uiso 1 1 calc R U . . .
H11B H 0.974497 0.950434 0.821707 0.040 Uiso 1 1 calc R U . . .
H11C H 0.818971 0.943840 0.769685 0.040 Uiso 1 1 calc R U . . .
C10 C 1.08033(19) 0.8946(2) 0.65936(14) 0.0291(4) Uani 1 1 d . . . . .
H10A H 1.076219 0.828816 0.593630 0.044 Uiso 1 1 calc R U . . .
H10B H 1.121720 0.868354 0.715835 0.044 Uiso 1 1 calc R U . . .
H10C H 1.145610 1.002109 0.666540 0.044 Uiso 1 1 calc R U . . .
C2 C 0.90188(17) 0.66443(17) 0.80371(11) 0.0165(3) Uani 1 1 d . . . . .
Si1 Si 0.75701(5) 0.48426(5) 0.38610(4) 0.02436(13) Uani 1 1 d D . . . .
N1 N 0.81584(14) 0.70662(14) 0.64007(9) 0.0173(3) Uani 1 1 d . . . . .
Al1 Al 0.64743(5) 0.53519(5) 0.53085(3) 0.01577(12) Uani 1 1 d . . . . .
H1 H 0.5410(18) 0.6220(19) 0.5228(13) 0.021(4) Uiso 1 1 d . . . . .
C1 C 0.80707(16) 0.61668(17) 0.69759(11) 0.0169(3) Uani 1 1 d . . . . .
N2 N 0.69172(15) 0.47520(14) 0.64800(10) 0.0204(3) Uani 1 1 d D U . . .
C12 C 0.65802(18) 0.33359(17) 0.67526(12) 0.0206(3) Uani 1 1 d D U . . .
C13 C 0.7762(3) 0.2833(3) 0.6550(2) 0.0304(6) Uani 0.804(3) 1 d D U P A 1
H13A H 0.782448 0.273665 0.583822 0.046 Uiso 0.804(3) 1 calc R U P A 1
H13B H 0.747885 0.184137 0.666209 0.046 Uiso 0.804(3) 1 calc R U P A 1
H13C H 0.875052 0.359547 0.701905 0.046 Uiso 0.804(3) 1 calc R U P A 1
C14 C 0.6481(3) 0.3503(2) 0.78887(16) 0.0260(5) Uani 0.804(3) 1 d D U P A 1
H14A H 0.586745 0.401920 0.805752 0.039 Uiso 0.804(3) 1 calc R U P A 1
H14B H 0.750508 0.410896 0.835056 0.039 Uiso 0.804(3) 1 calc R U P A 1
H14C H 0.600950 0.248504 0.797085 0.039 Uiso 0.804(3) 1 calc R U P A 1
C15 C 0.5021(2) 0.2118(2) 0.60741(17) 0.0274(5) Uani 0.804(3) 1 d D U P A 1
H15A H 0.503650 0.195487 0.535004 0.041 Uiso 0.804(3) 1 calc R U P A 1
H15B H 0.426237 0.245709 0.620765 0.041 Uiso 0.804(3) 1 calc R U P A 1
H15C H 0.476120 0.115644 0.622778 0.041 Uiso 0.804(3) 1 calc R U P A 1
C13A C 0.6099(10) 0.2001(9) 0.5677(6) 0.026(2) Uani 0.196(3) 1 d D U P A 2
H13X H 0.529100 0.199268 0.519150 0.039 Uiso 0.196(3) 1 calc R U P A 2
H13Y H 0.573221 0.100626 0.579568 0.039 Uiso 0.196(3) 1 calc R U P A 2
H13Z H 0.698158 0.219338 0.539076 0.039 Uiso 0.196(3) 1 calc R U P A 2
C14A C 0.7892(9) 0.3246(9) 0.7374(7) 0.029(2) Uani 0.196(3) 1 d D U P A 2
H14X H 0.756034 0.219572 0.738854 0.043 Uiso 0.196(3) 1 calc R U P A 2
H14Y H 0.821501 0.394386 0.807756 0.043 Uiso 0.196(3) 1 calc R U P A 2
H14Z H 0.874492 0.354172 0.705455 0.043 Uiso 0.196(3) 1 calc R U P A 2
C15A C 0.5269(9) 0.3065(10) 0.7171(7) 0.031(2) Uani 0.196(3) 1 d D U P A 2
H15X H 0.447097 0.306823 0.668414 0.046 Uiso 0.196(3) 1 calc R U P A 2
H15Y H 0.556337 0.387475 0.782375 0.046 Uiso 0.196(3) 1 calc R U P A 2
H15Z H 0.488758 0.206910 0.728876 0.046 Uiso 0.196(3) 1 calc R U P A 2
C17 C 0.53550(18) 0.21770(18) 0.22087(12) 0.0208(3) Uani 1 1 d . . . . .
C18 C 0.44892(18) 0.13562(19) 0.12051(13) 0.0232(4) Uani 1 1 d . . . . .
H18 H 0.384690 0.028665 0.103368 0.028 Uiso 1 1 calc R U . . .
C19 C 0.45264(18) 0.2038(2) 0.04435(13) 0.0251(4) Uani 1 1 d . . . . .
C20 C 0.54594(19) 0.3610(2) 0.07269(13) 0.0260(4) Uani 1 1 d . . . . .
H20 H 0.549129 0.411334 0.022373 0.031 Uiso 1 1 calc R U . . .
C21 C 0.63493(18) 0.44695(19) 0.17281(14) 0.0248(4) Uani 1 1 d . . . . .
C22 C 0.7372(2) 0.6160(2) 0.19464(17) 0.0405(5) Uani 1 1 d . . . . .
H22A H 0.843150 0.635693 0.205121 0.061 Uiso 1 1 calc R U . . .
H22B H 0.724737 0.674693 0.256680 0.061 Uiso 1 1 calc R U . . .
H22C H 0.710012 0.647121 0.136272 0.061 Uiso 1 1 calc R U . . .
C23 C 0.5256(2) 0.1333(2) 0.29807(14) 0.0290(4) Uani 1 1 d . . . . .
H23A H 0.445961 0.026943 0.266677 0.044 Uiso 1 1 calc R U . . .
H23B H 0.501281 0.183030 0.357830 0.044 Uiso 1 1 calc R U . . .
H23C H 0.623265 0.134903 0.319985 0.044 Uiso 1 1 calc R U . . .
C24 C 0.3578(2) 0.1106(2) -0.06360(14) 0.0357(4) Uani 1 1 d . . . . .
H24A H 0.377203 0.176707 -0.107221 0.053 Uiso 1 1 calc R U . . .
H24B H 0.250107 0.065181 -0.064033 0.053 Uiso 1 1 calc R U . . .
H24C H 0.384356 0.028910 -0.090017 0.053 Uiso 1 1 calc R U . . .
C16 C 0.63248(17) 0.37665(18) 0.24939(12) 0.0207(3) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0406 0.0313 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 '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
C2 C3 C4 119.76(15) . .
C5 C4 C3 120.46(16) . .
C6 C7 C2 119.87(15) . .
C5 C6 C7 120.46(16) . .
C4 C5 C6 119.78(16) . .
N1 C8 C9 105.73(12) . .
N1 C8 C11 112.66(13) . .
C9 C8 C11 108.26(13) . .
N1 C8 C10 110.38(13) . .
C9 C8 C10 109.16(14) . .
C11 C8 C10 110.46(14) . .
C3 C2 C7 119.63(14) . .
C3 C2 C1 122.19(14) . .
C7 C2 C1 118.15(13) . .
H2Y Si1 H2X 102.7(11) . .
H2Y Si1 C16 107.9(8) . .
H2X Si1 C16 105.3(8) . .
H2Y Si1 Al1 109.8(8) . .
H2X Si1 Al1 108.4(8) . .
C16 Si1 Al1 121.16(5) . .
C1 N1 C8 129.46(13) . .
C1 N1 Al1 90.49(10) . .
C8 N1 Al1 140.05(10) . .
H1 Al1 H1 77.0(9) . 2_666
H1 Al1 N2 123.3(6) . .
H1 Al1 N2 95.5(5) 2_666 .
H1 Al1 N1 95.7(6) . .
H1 Al1 N1 155.4(5) 2_666 .
N2 Al1 N1 68.60(6) . .
H1 Al1 C1 113.6(6) . .
H1 Al1 C1 128.0(5) 2_666 .
N2 Al1 C1 34.59(6) . .
N1 Al1 C1 34.02(5) . .
H1 Al1 Si1 118.0(6) . .
H1 Al1 Si1 98.5(5) 2_666 .
N2 Al1 Si1 118.66(5) . .
N1 Al1 Si1 105.58(5) . .
C1 Al1 Si1 116.15(4) . .
H1 Al1 Al1 40.4(6) . 2_666
H1 Al1 Al1 36.6(5) 2_666 2_666
N2 Al1 Al1 113.57(5) . 2_666
N1 Al1 Al1 131.70(5) . 2_666
C1 Al1 Al1 130.92(5) . 2_666
Si1 Al1 Al1 112.72(3) . 2_666
N1 C1 N2 109.58(13) . .
N1 C1 C2 126.14(14) . .
N2 C1 C2 124.17(14) . .
N1 C1 Al1 55.49(8) . .
N2 C1 Al1 54.12(8) . .
C2 C1 Al1 177.70(11) . .
C1 N2 C12 127.50(13) . .
C1 N2 Al1 91.29(10) . .
C12 N2 Al1 139.28(10) . .
C15A C12 N2 104.3(4) . .
N2 C12 C13 109.64(14) . .
N2 C12 C15 107.04(14) . .
C13 C12 C15 110.06(16) . .
C15A C12 C14A 116.7(5) . .
N2 C12 C14A 117.9(3) . .
N2 C12 C14 113.66(14) . .
C13 C12 C14 109.77(16) . .
C15 C12 C14 106.57(15) . .
C15A C12 C13A 109.6(5) . .
N2 C12 C13A 105.6(3) . .
C14A C12 C13A 102.1(5) . .
C18 C17 C16 120.55(15) . .
C18 C17 C23 118.62(15) . .
C16 C17 C23 120.82(15) . .
C19 C18 C17 122.40(16) . .
C18 C19 C20 117.18(16) . .
C18 C19 C24 120.71(17) . .
C20 C19 C24 122.11(17) . .
C19 C20 C21 121.90(16) . .
C20 C21 C16 120.64(16) . .
C20 C21 C22 117.74(16) . .
C16 C21 C22 121.59(16) . .
C21 C16 C17 117.31(15) . .
C21 C16 Si1 123.13(12) . .
C17 C16 Si1 119.54(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C3 C2 1.385(2) .
C3 C4 1.387(2) .
C4 C5 1.377(3) .
C7 C6 1.381(2) .
C7 C2 1.392(2) .
C6 C5 1.378(2) .
C8 N1 1.475(2) .
C8 C9 1.525(2) .
C8 C11 1.527(2) .
C8 C10 1.529(2) .
C2 C1 1.490(2) .
Si1 H2Y 1.414(16) .
Si1 H2X 1.425(16) .
Si1 C16 1.9025(18) .
Si1 Al1 2.4602(8) .
N1 C1 1.327(2) .
N1 Al1 1.9543(16) .
Al1 H1 1.653(16) .
Al1 H1 1.796(17) 2_666
Al1 N2 1.9220(14) .
Al1 C1 2.3716(17) .
Al1 Al1 2.7004(12) 2_666
C1 N2 1.347(2) .
N2 C12 1.482(2) .
C12 C15A 1.453(8) .
C12 C13 1.508(3) .
C12 C15 1.522(3) .
C12 C14A 1.526(7) .
C12 C14 1.562(3) .
C12 C13A 1.617(7) .
C17 C18 1.386(2) .
C17 C16 1.411(2) .
C17 C23 1.505(2) .
C18 C19 1.385(2) .
C19 C20 1.391(3) .
C19 C24 1.501(2) .
C20 C21 1.394(3) .
C21 C16 1.405(2) .
C21 C22 1.512(3) .
