#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:48:26 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179207 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/39/4313975.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_4313975
loop_
_publ_author_name
'Marcus Schiefer'
'N. Dastagiri Reddy'
'Hans-Jürgen Ahn'
'Andreas Stasch'
'Herbert W. Roesky'
'A. Christine Schlicker'
'Hans-Georg Schmidt'
'Mathias Noltemeyer'
'Denis Vidovic'
_publ_section_title
;
 Neutral and Ionic Aluminum, Gallium, and Indium Compounds Carrying Two or
 Three Terminal Ethynyl Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4970
_journal_page_last               4976
_journal_paper_doi               10.1021/ic0342806
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C27 H49 In N'
_chemical_formula_weight         502.49
_chemical_name_systematic
;
compound 9
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   15.659(2)
_cell_length_b                   15.659(2)
_cell_length_c                   14.032(3)
_cell_measurement_reflns_used    16974
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.6
_cell_volume                     2979.7(8)
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe-IPDS 2'
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16974
_diffrn_reflns_theta_full        24.82
_diffrn_reflns_theta_max         24.82
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  0.8557
_exptl_absorpt_correction_T_min  0.7944
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1708
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0335P)²+2.1751P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                1331
_reflns_number_total             1708
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ic0342806_09.cif
_cod_data_source_block           schiefer9
_cod_database_code               4313975
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, -z-1/2'
'x-y, -y, -z-1/2'
'-x, -x+y, -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
In1 In 0.3333 -0.3333 -0.07711(2) 0.03379(14) Uani 1 3 d S . .
C1 C 0.4691(2) -0.2039(2) -0.0481(2) 0.0401(6) Uani 1 1 d U . .
C2 C 0.5470(2) -0.1290(2) -0.0428(2) 0.0445(7) Uani 1 1 d DU A .
C3 C 0.6430(2) -0.0361(2) -0.0388(3) 0.0554(8) Uani 1 1 d DU . .
C31 C 0.7193(4) -0.0477(4) -0.0939(6) 0.098(2) Uani 0.729(5) 1 d PDU A 1
H31A H 0.7826 0.0140 -0.0911 0.147 Uiso 0.729(5) 1 calc PR A 1
H31B H 0.6983 -0.0634 -0.1605 0.147 Uiso 0.729(5) 1 calc PR A 1
H31C H 0.7265 -0.1011 -0.0660 0.147 Uiso 0.729(5) 1 calc PR A 1
C32 C 0.6343(4) 0.0473(3) -0.0836(6) 0.0916(18) Uani 0.729(5) 1 d PDU A 1
H32A H 0.6982 0.1083 -0.0804 0.137 Uiso 0.729(5) 1 calc PR A 1
H32B H 0.5849 0.0561 -0.0490 0.137 Uiso 0.729(5) 1 calc PR A 1
H32C H 0.6142 0.0314 -0.1504 0.137 Uiso 0.729(5) 1 calc PR A 1
C33 C 0.6740(6) -0.0140(7) 0.0631(5) 0.165(4) Uani 0.729(5) 1 d PDU A 1
H33A H 0.7374 0.0475 0.0670 0.248 Uiso 0.729(5) 1 calc PR A 1
H33B H 0.6806 -0.0681 0.0901 0.248 Uiso 0.729(5) 1 calc PR A 1
H33C H 0.6242 -0.0069 0.0989 0.248 Uiso 0.729(5) 1 calc PR A 1
N1 N 0.3333 -0.3333 -0.2417(3) 0.0550(11) Uani 1 3 d SD . .
C4 C 0.2299(5) -0.3797(5) -0.2780(4) 0.070(2) Uani 0.560(11) 1 d PDU B 1
H4A H 0.2306 -0.3711 -0.3480 0.085 Uiso 0.560(11) 1 calc PR B 1
H4B H 0.1963 -0.3468 -0.2489 0.085 Uiso 0.560(11) 1 calc PR B 1
C41 C 0.1719(3) -0.4931(3) -0.2527(3) 0.0935(14) Uani 1 1 d DU . .
H41A H 0.1041 -0.5226 -0.2763 0.140 Uiso 0.560(11) 1 calc PR B 1
H41B H 0.1711 -0.5013 -0.1834 0.140 Uiso 0.560(11) 1 calc PR B 1
H41C H 0.2045 -0.5257 -0.2827 0.140 Uiso 0.560(11) 1 calc PR B 1
H41D H 0.1410 -0.5614 -0.2751 0.140 Uiso 0.440(11) 1 calc PR B 2
H41E H 0.1409 -0.4596 -0.2842 0.140 Uiso 0.440(11) 1 calc PR B 2
H41F H 0.1632 -0.4925 -0.1836 0.140 Uiso 0.440(11) 1 calc PR B 2
C4' C 0.2864(7) -0.4374(7) -0.2774(6) 0.075(3) Uani 0.440(11) 1 d PDU B 2
H4'1 H 0.3179 -0.4717 -0.2469 0.090 Uiso 0.440(11) 1 calc PR B 2
H4'2 H 0.2956 -0.4375 -0.3472 0.090 Uiso 0.440(11) 1 calc PR B 2
C31' C 0.6377(11) 0.0371(9) 0.0237(14) 0.098(2) Uani 0.271(5) 1 d PDU A 2
H31D H 0.7021 0.0977 0.0250 0.147 Uiso 0.271(5) 1 calc PR A 2
H31E H 0.6198 0.0103 0.0884 0.147 Uiso 0.271(5) 1 calc PR A 2
H31F H 0.5878 0.0518 -0.0007 0.147 Uiso 0.271(5) 1 calc PR A 2
C32' C 0.7209(9) -0.0560(10) 0.0008(15) 0.0916(18) Uani 0.271(5) 1 d PDU A 2
H32D H 0.7842 0.0058 0.0033 0.137 Uiso 0.271(5) 1 calc PR A 2
H32E H 0.7270 -0.1032 -0.0403 0.137 Uiso 0.271(5) 1 calc PR A 2
H32F H 0.7021 -0.0834 0.0652 0.137 Uiso 0.271(5) 1 calc PR A 2
C33' C 0.6724(15) 0.0024(16) -0.1388(9) 0.165(4) Uani 0.271(5) 1 d PDU A 2
H33D H 0.7358 0.0641 -0.1375 0.248 Uiso 0.271(5) 1 calc PR A 2
H33E H 0.6221 0.0145 -0.1666 0.248 Uiso 0.271(5) 1 calc PR A 2
H33F H 0.6785 -0.0464 -0.1774 0.248 Uiso 0.271(5) 1 calc PR A 2
C1S' C -0.104(6) -0.012(5) 1.209(7) 0.42(4) Uani 0.17 1 d PDU C -2
H1S4 H -0.0656 0.0176 1.2674 0.624 Uiso 0.17 1 calc PR C -2
H1S5 H -0.1559 -0.0796 1.2223 0.624 Uiso 0.17 1 calc PR C -2
H1S6 H -0.1334 0.0271 1.1876 0.624 Uiso 0.17 1 calc PR C -2
C2S' C -0.035(6) -0.012(6) 1.131(6) 0.42(4) Uani 0.17 1 d PDU C -2
H2S3 H 0.0341 0.0376 1.1458 0.499 Uiso 0.17 1 calc PR C -2
H2S4 H -0.0399 -0.0778 1.1287 0.499 Uiso 0.17 1 calc PR C -2
C3S' C -0.064(6) 0.011(5) 1.034(6) 0.42(4) Uani 0.17 1 d PDU C -2
H3S3 H -0.0574 0.0770 1.0354 0.499 Uiso 0.17 1 calc PR C -2
H3S4 H -0.1340 -0.0381 1.0199 0.499 Uiso 0.17 1 calc PR C -2
C4S' C 0.002(7) 0.007(6) 0.955(6) 0.42(4) Uani 0.17 1 d PDU C -2
H4S3 H 0.0725 0.0524 0.9711 0.499 Uiso 0.17 1 calc PR C -2
H4S4 H -0.0078 -0.0607 0.9503 0.499 Uiso 0.17 1 calc PR C -2
C5S' C -0.023(8) 0.037(6) 0.859(6) 0.42(4) Uani 0.17 1 d PDU C -2
H5S3 H -0.0935 -0.0076 0.8445 0.500 Uiso 0.17 1 calc PR C -2
H5S4 H -0.0116 0.1050 0.8642 0.500 Uiso 0.17 1 calc PR C -2
C6S' C 0.041(8) 0.032(6) 0.779(6) 0.42(4) Uani 0.17 1 d PDU C -2
H6S4 H -0.0002 -0.0023 0.7241 0.625 Uiso 0.50 3 calc SPR C -2
H6S5 H 0.0734 -0.0044 0.8019 0.625 Uiso 0.17 1 calc PR C -2
H6S6 H 0.0916 0.0987 0.7609 0.625 Uiso 0.17 1 calc PR C -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'
In In -0.7276 1.3100 '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
C1 In1 C1 116.40(5) 2_545 3_655 ?
C1 In1 C1 116.40(5) 2_545 . ?
C1 In1 C1 116.40(5) 3_655 . ?
C1 In1 N1 101.08(8) 2_545 . ?
C1 In1 N1 101.08(8) 3_655 . ?
C1 In1 N1 101.08(8) . . ?
C2 C1 In1 172.5(3) . . ?
C1 C2 C3 178.6(4) . . ?
C31' C3 C2 111.2(6) . . ?
C31' C3 C33 52.4(8) . . ?
C2 C3 C33 108.4(3) . . ?
C31' C3 C33' 111.6(12) . . ?
C2 C3 C33' 108.4(7) . . ?
C33 C3 C33' 143.2(7) . . ?
C31' C3 C32' 107.8(10) . . ?
C2 C3 C32' 109.9(5) . . ?
C33 C3 C32' 59.5(8) . . ?
C33' C3 C32' 108.0(12) . . ?
C31' C3 C31 138.8(6) . . ?
C2 C3 C31 109.8(3) . . ?
C33 C3 C31 109.5(6) . . ?
C33' C3 C31 57.8(12) . . ?
C32' C3 C31 52.6(7) . . ?
C31' C3 C32 61.0(8) . . ?
C2 C3 C32 110.3(3) . . ?
C33 C3 C32 110.9(6) . . ?
C33' C3 C32 53.8(12) . . ?
C32' C3 C32 139.6(6) . . ?
C31 C3 C32 108.0(4) . . ?
C4 N1 C4 109.0(3) 2_545 . ?
C4 N1 C4 109.0(3) 2_545 3_655 ?
C4 N1 C4 109.0(3) . 3_655 ?
C4 N1 C4' 62.3(5) 2_545 2_545 ?
C4 N1 C4' 140.0(5) . 2_545 ?
C4 N1 C4' 50.0(4) 3_655 2_545 ?
C4 N1 C4' 50.0(4) 2_545 . ?
C4 N1 C4' 62.3(5) . . ?
C4 N1 C4' 140.0(5) 3_655 . ?
C4' N1 C4' 109.4(4) 2_545 . ?
C4 N1 C4' 140.0(5) 2_545 3_655 ?
C4 N1 C4' 49.9(4) . 3_655 ?
C4 N1 C4' 62.3(5) 3_655 3_655 ?
C4' N1 C4' 109.4(4) 2_545 3_655 ?
C4' N1 C4' 109.4(4) . 3_655 ?
C4 N1 In1 109.9(3) 2_545 . ?
C4 N1 In1 109.9(3) . . ?
C4 N1 In1 109.9(3) 3_655 . ?
C4' N1 In1 109.5(4) 2_545 . ?
C4' N1 In1 109.5(4) . . ?
C4' N1 In1 109.5(4) 3_655 . ?
N1 C4 C41 110.1(5) . . ?
C4 C41 C4' 58.5(5) . . ?
N1 C4' C41 109.2(6) . . ?
C3S' C2S' C1S' 109.8(11) . . ?
C2S' C3S' C4S' 109.8(11) . . ?
C5S' C4S' C3S' 109.2(11) . . ?
C6S' C5S' C4S' 110.2(11) . . ?
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
In1 C1 2.118(3) 2_545 ?
In1 C1 2.118(3) 3_655 ?
In1 C1 2.118(3) . ?
In1 N1 2.309(4) . ?
C1 C2 1.200(4) . ?
C2 C3 1.480(4) . ?
C3 C31' 1.478(11) . ?
C3 C33 1.493(7) . ?
C3 C33' 1.505(11) . ?
C3 C32' 1.508(11) . ?
C3 C31 1.508(6) . ?
C3 C32 1.516(6) . ?
N1 C4 1.495(7) 2_545 ?
N1 C4 1.495(7) . ?
N1 C4 1.495(7) 3_655 ?
N1 C4' 1.500(8) 2_545 ?
N1 C4' 1.500(8) . ?
N1 C4' 1.500(8) 3_655 ?
C4 C41 1.578(8) . ?
C41 C4' 1.591(10) . ?
C1S' C2S' 1.540(7) . ?
C2S' C3S' 1.538(7) . ?
C3S' C4S' 1.540(7) . ?
C4S' C5S' 1.540(7) . ?
C5S' C6S' 1.539(7) . ?
