#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:12:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179444 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/41/4334184.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_4334184
loop_
_publ_author_name
'Sandra González-Gallardo'
'Aracely S. Cruz-Zavala'
'Vojtech Jancik'
'Fernando Cortés-Guzmán'
'Mónica Moya-Cabrera'
_publ_section_title
;
 Preparation of Telluro- and Selenoalumoxanes under Mild Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2793
_journal_page_last               2795
_journal_paper_doi               10.1021/ic302588f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C46 H60 Al2 N4 O Se2, 2(C7 H8)'
_chemical_formula_sum            'C60 H76 Al2 N4 O Se2'
_chemical_formula_weight         1081.13
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.111(3)
_cell_length_b                   13.118(2)
_cell_length_c                   20.256(2)
_cell_measurement_reflns_used    6422
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      1.83
_cell_volume                     5609.6(13)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20540
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  0.6793
_exptl_absorpt_correction_T_min  0.5924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5143
_refine_ls_number_restraints     554
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0416
_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)+(0.0557P)²+1.2606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                3907
_reflns_number_total             5143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302588f_si_002_1.cif
_cod_data_source_block           Compound4
_cod_original_cell_volume        5610(1)
_cod_database_code               4334184
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
Se1 Se 0.694902(13) 0.60564(3) 0.170533(15) 0.04724(12) Uani 1 1 d . . .
H1 H 0.7446(17) 0.576(2) 0.1806(15) 0.071 Uiso 1 1 d . . .
N1 N 0.64177(8) 0.61344(14) 0.33410(10) 0.0262(4) Uani 1 1 d . . .
Al1 Al 0.68162(3) 0.69760(5) 0.27028(4) 0.02406(17) Uani 1 1 d . . .
N2 N 0.61231(8) 0.78835(14) 0.25791(9) 0.0255(4) Uani 1 1 d . . .
C3 C 0.55283(10) 0.75977(19) 0.27054(12) 0.0304(6) Uani 1 1 d . . .
C4 C 0.62316(10) 0.89149(17) 0.23388(12) 0.0268(5) Uani 1 1 d . . .
C5 C 0.62005(11) 0.91386(18) 0.16663(12) 0.0284(5) Uani 1 1 d . . .
C6 C 0.69509(10) 0.60413(17) 0.44122(13) 0.0273(5) Uani 1 1 d . . .
C7 C 0.57874(10) 0.60555(18) 0.33811(12) 0.0293(6) Uani 1 1 d . . .
C8 C 0.64866(11) 1.08967(19) 0.19101(13) 0.0318(6) Uani 1 1 d . . .
O1 O 0.7500 0.7500 0.29769(11) 0.0260(5) Uani 1 2 d S . .
C10 C 0.63744(10) 0.96738(19) 0.28037(12) 0.0289(5) Uani 1 1 d . . .
C11 C 0.69895(10) 0.45730(18) 0.36806(13) 0.0312(6) Uani 1 1 d . . .
C12 C 0.64986(11) 1.0652(2) 0.25750(13) 0.0325(6) Uani 1 1 d . . .
H12A H 0.6595 1.1172 0.2886 0.039 Uiso 1 1 calc R . .
C13 C 0.49862(11) 0.8291(2) 0.25323(14) 0.0412(7) Uani 1 1 d . . .
H13A H 0.4996 0.8439 0.2058 0.062 Uiso 1 1 calc R . .
H13B H 0.5025 0.8928 0.2781 0.062 Uiso 1 1 calc R . .
H13C H 0.4585 0.7957 0.2644 0.062 Uiso 1 1 calc R . .
C14 C 0.73096(11) 0.55134(18) 0.48665(12) 0.0304(6) Uani 1 1 d . . .
H14A H 0.7418 0.5836 0.5271 0.036 Uiso 1 1 calc R . .
C15 C 0.67351(12) 0.71125(18) 0.45509(13) 0.0335(6) Uani 1 1 d . . .
H15A H 0.6903 0.7571 0.4212 0.050 Uiso 1 1 calc R . .
H15B H 0.6890 0.7326 0.4985 0.050 Uiso 1 1 calc R . .
H15C H 0.6271 0.7138 0.4546 0.050 Uiso 1 1 calc R . .
C16 C 0.53792(10) 0.66854(19) 0.30272(13) 0.0323(6) Uani 1 1 d . . .
H16A H 0.4950 0.6471 0.3001 0.039 Uiso 1 1 calc R . .
C17 C 0.54975(11) 0.5299(2) 0.38492(14) 0.0391(6) Uani 1 1 d . . .
H17A H 0.5668 0.4619 0.3758 0.059 Uiso 1 1 calc R . .
H17B H 0.5037 0.5293 0.3790 0.059 Uiso 1 1 calc R . .
H17C H 0.5599 0.5493 0.4304 0.059 Uiso 1 1 calc R . .
C18 C 0.63368(10) 1.01305(19) 0.14682(13) 0.0313(6) Uani 1 1 d . . .
H18A H 0.6327 1.0288 0.1010 0.038 Uiso 1 1 calc R . .
C19 C 0.79244(14) 0.3970(2) 0.52473(16) 0.0488(8) Uani 1 1 d . . .
H19A H 0.7774 0.4124 0.5694 0.073 Uiso 1 1 calc R . .
H19B H 0.8365 0.4193 0.5201 0.073 Uiso 1 1 calc R . .
H19C H 0.7898 0.3234 0.5170 0.073 Uiso 1 1 calc R . .
C20 C 0.63962(12) 0.9435(2) 0.35295(13) 0.0361(6) Uani 1 1 d . . .
H20A H 0.6419 1.0072 0.3781 0.054 Uiso 1 1 calc R . .
H20B H 0.6770 0.9018 0.3625 0.054 Uiso 1 1 calc R . .
H20C H 0.6013 0.9061 0.3655 0.054 Uiso 1 1 calc R . .
C21 C 0.73536(11) 0.40765(18) 0.41562(14) 0.0355(6) Uani 1 1 d . . .
H21A H 0.7495 0.3403 0.4068 0.043 Uiso 1 1 calc R . .
C23 C 0.67955(10) 0.55693(18) 0.38166(13) 0.0268(5) Uani 1 1 d . . .
C24 C 0.68219(13) 0.4030(2) 0.30499(16) 0.0439(7) Uani 1 1 d . . .
H24A H 0.6360 0.3991 0.3007 0.066 Uiso 1 1 calc R . .
H24B H 0.6999 0.3339 0.3058 0.066 Uiso 1 1 calc R . .
H24C H 0.6997 0.4405 0.2674 0.066 Uiso 1 1 calc R . .
C26 C 0.75182(11) 0.45206(18) 0.47508(13) 0.0334(6) Uani 1 1 d . . .
C27 C 0.66380(14) 1.1963(2) 0.16724(14) 0.0444(7) Uani 1 1 d . . .
H27A H 0.6961 1.1929 0.1325 0.067 Uiso 1 1 calc R . .
H27B H 0.6798 1.2370 0.2042 0.067 Uiso 1 1 calc R . .
H27C H 0.6253 1.2280 0.1496 0.067 Uiso 1 1 calc R . .
C28 C 0.60332(12) 0.8353(2) 0.11587(13) 0.0414(7) Uani 1 1 d . . .
H28A H 0.5991 0.8680 0.0726 0.062 Uiso 1 1 calc R . .
H28B H 0.5631 0.8028 0.1278 0.062 Uiso 1 1 calc R . .
H28C H 0.6368 0.7836 0.1140 0.062 Uiso 1 1 calc R . .
C100 C 0.5218(4) 0.9484(7) 0.6199(4) 0.081(3) Uani 0.461(3) 1 d PDU A 1
H10A H 0.4980 0.9476 0.6614 0.121 Uiso 0.461(3) 1 calc PR A 1
H10B H 0.5185 1.0159 0.5995 0.121 Uiso 0.461(3) 1 calc PR A 1
H10C H 0.5664 0.9330 0.6288 0.121 Uiso 0.461(3) 1 calc PR A 1
C101 C 0.4961(3) 0.8725(5) 0.5755(3) 0.0490(16) Uani 0.461(3) 1 d PDU A 1
C102 C 0.4467(12) 0.812(2) 0.5963(9) 0.0570(19) Uani 0.461(3) 1 d PDU A 1
H102 H 0.4302 0.8206 0.6396 0.068 Uiso 0.461(3) 1 calc PR A 1
C103 C 0.4205(5) 0.7386(7) 0.5557(5) 0.062(2) Uani 0.461(3) 1 d PDU A 1
H103 H 0.3850 0.7000 0.5699 0.074 Uiso 0.461(3) 1 calc PR A 1
C104 C 0.4467(6) 0.7223(10) 0.4940(5) 0.063(2) Uani 0.461(3) 1 d PDU A 1
H104 H 0.4306 0.6697 0.4665 0.076 Uiso 0.461(3) 1 calc PR A 1
C105 C 0.4963(7) 0.7823(11) 0.4723(5) 0.057(2) Uani 0.461(3) 1 d PDU A 1
H105 H 0.5139 0.7721 0.4297 0.068 Uiso 0.461(3) 1 calc PR A 1
C106 C 0.5195(5) 0.8560(9) 0.5125(4) 0.0489(18) Uani 0.461(3) 1 d PDU A 1
H106 H 0.5531 0.8979 0.4969 0.059 Uiso 0.461(3) 1 calc PR A 1
C200 C 0.5631(5) 0.9296(8) 0.5389(6) 0.074(3) Uani 0.355(5) 1 d PDU B 2
H20D H 0.5854 0.9314 0.4965 0.111 Uiso 0.355(5) 1 calc PR B 2
H20E H 0.5926 0.9085 0.5737 0.111 Uiso 0.355(5) 1 calc PR B 2
H20F H 0.5465 0.9976 0.5491 0.111 Uiso 0.355(5) 1 calc PR B 2
C201 C 0.5112(6) 0.8577(11) 0.5352(5) 0.056(2) Uani 0.355(5) 1 d PDU B 2
C202 C 0.5017(10) 0.8041(18) 0.4775(7) 0.057(2) Uani 0.355(5) 1 d PDU B 2
H202 H 0.5278 0.8183 0.4404 0.069 Uiso 0.355(5) 1 calc PR B 2
C203 C 0.4553(6) 0.7305(11) 0.4723(5) 0.049(2) Uani 0.355(5) 1 d PDU B 2
H203 H 0.4503 0.6929 0.4326 0.059 Uiso 0.355(5) 1 calc PR B 2
C204 C 0.4163(5) 0.7123(9) 0.5260(5) 0.048(2) Uani 0.355(5) 1 d PDU B 2
H204 H 0.3841 0.6618 0.5232 0.058 Uiso 0.355(5) 1 calc PR B 2
C205 C 0.4239(6) 0.7673(9) 0.5835(5) 0.053(2) Uani 0.355(5) 1 d PDU B 2
H205 H 0.3967 0.7554 0.6202 0.064 Uiso 0.355(5) 1 calc PR B 2
C206 C 0.4704(6) 0.8384(10) 0.5873(5) 0.062(2) Uani 0.355(5) 1 d PDU B 2
H206 H 0.4752 0.8762 0.6270 0.075 Uiso 0.355(5) 1 calc PR B 2
C300 C 0.4212(11) 0.696(2) 0.4969(11) 0.063(5) Uani 0.184(4) 1 d PDU C 3
H30A H 0.4402 0.6783 0.4543 0.095 Uiso 0.184(4) 1 calc PR C 3
H30B H 0.3787 0.7244 0.4897 0.095 Uiso 0.184(4) 1 calc PR C 3
H30C H 0.4180 0.6349 0.5244 0.095 Uiso 0.184(4) 1 calc PR C 3
C301 C 0.4603(7) 0.7710(11) 0.5298(7) 0.055(2) Uani 0.184(4) 1 d PDU C 3
C302 C 0.5100(12) 0.816(2) 0.4968(9) 0.052(3) Uani 0.184(4) 1 d PDU C 3
H302 H 0.5193 0.7944 0.4531 0.063 Uiso 0.184(4) 1 calc PR C 3
C303 C 0.5466(9) 0.8908(15) 0.5254(9) 0.054(3) Uani 0.184(4) 1 d PDU C 3
H303 H 0.5814 0.9194 0.5021 0.065 Uiso 0.184(4) 1 calc PR C 3
C304 C 0.5321(8) 0.9237(13) 0.5884(8) 0.057(3) Uani 0.184(4) 1 d PDU C 3
H304 H 0.5556 0.9775 0.6080 0.069 Uiso 0.184(4) 1 calc PR C 3
C305 C 0.4831(7) 0.8781(12) 0.6229(7) 0.057(3) Uani 0.184(4) 1 d PDU C 3
H305 H 0.4752 0.8962 0.6675 0.069 Uiso 0.184(4) 1 calc PR C 3
C306 C 0.446(3) 0.808(6) 0.593(2) 0.057(3) Uani 0.184(4) 1 d PDU C 3
H306 H 0.4101 0.7825 0.6149 0.068 Uiso 0.184(4) 1 calc PR C 3
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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
H1 Se1 Al1 97.5(15) .
C7 N1 C23 117.79(19) .
C7 N1 Al1 121.86(16) .
C23 N1 Al1 120.33(14) .
O1 Al1 N1 113.03(9) .
O1 Al1 N2 116.42(7) .
N1 Al1 N2 96.47(8) .
O1 Al1 Se1 112.67(7) .
N1 Al1 Se1 109.71(7) .
N2 Al1 Se1 107.29(6) .
C3 N2 C4 118.22(19) .
C3 N2 Al1 121.49(16) .
C4 N2 Al1 120.29(13) .
N2 C3 C16 122.8(2) .
N2 C3 C13 120.1(2) .
C16 C3 C13 117.1(2) .
C5 C4 C10 121.1(2) .
C5 C4 N2 121.0(2) .
C10 C4 N2 118.0(2) .
C18 C5 C4 117.9(2) .
C18 C5 C28 119.6(2) .
C4 C5 C28 122.5(2) .
C14 C6 C23 118.9(2) .
C14 C6 C15 120.7(2) .
C23 C6 C15 120.3(2) .
N1 C7 C16 122.6(2) .
N1 C7 C17 119.7(2) .
C16 C7 C17 117.7(2) .
C18 C8 C12 117.7(2) .
C18 C8 C27 120.9(2) .
C12 C8 C27 121.3(2) .
Al1 O1 Al1 141.71(15) 2_665
C12 C10 C4 118.2(2) .
C12 C10 C20 120.8(2) .
C4 C10 C20 121.0(2) .
C21 C11 C23 117.5(2) .
C21 C11 C24 119.7(2) .
C23 C11 C24 122.8(2) .
C8 C12 C10 122.3(2) .
C6 C14 C26 122.0(2) .
C7 C16 C3 127.5(2) .
C8 C18 C5 122.7(2) .
C26 C21 C11 123.0(2) .
C6 C23 C11 121.1(2) .
C6 C23 N1 118.4(2) .
C11 C23 N1 120.5(2) .
C21 C26 C14 117.4(2) .
C21 C26 C19 121.5(2) .
C14 C26 C19 121.0(2) .
C102 C101 C106 117.5(7) .
C102 C101 C100 119.4(6) .
C106 C101 C100 123.0(7) .
C101 C102 C103 121.5(7) .
C102 C103 C104 119.1(8) .
C105 C104 C103 120.1(8) .
C106 C105 C104 119.4(7) .
C105 C106 C101 122.3(7) .
C202 C201 C206 117.6(8) .
C202 C201 C200 119.1(8) .
C206 C201 C200 123.3(8) .
C201 C202 C203 121.6(8) .
C202 C203 C204 118.9(9) .
C205 C204 C203 120.2(9) .
C206 C205 C204 119.5(8) .
C205 C206 C201 122.1(8) .
C302 C301 C306 117.2(9) .
C302 C301 C300 120.1(9) .
C306 C301 C300 122.4(9) .
C301 C302 C303 121.9(9) .
C302 C303 C304 119.1(10) .
C303 C304 C305 119.8(9) .
C306 C305 C304 119.6(9) .
C305 C306 C301 122.1(10) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 H1 1.14(4) .
Se1 Al1 2.3699(8) .
N1 C7 1.337(3) .
N1 C23 1.454(3) .
N1 Al1 1.897(2) .
Al1 O1 1.6925(10) .
Al1 N2 1.9029(19) .
N2 C3 1.335(3) .
N2 C4 1.456(3) .
C3 C16 1.399(3) .
C3 C13 1.503(3) .
C4 C5 1.395(3) .
C4 C10 1.403(3) .
C5 C18 1.392(3) .
C5 C28 1.498(3) .
C6 C14 1.378(3) .
C6 C23 1.395(3) .
C6 C15 1.504(3) .
C7 C16 1.393(3) .
C7 C17 1.503(3) .
C8 C18 1.383(4) .
C8 C12 1.385(4) .
C8 C27 1.513(4) .
O1 Al1 1.6926(10) 2_665
C10 C12 1.389(4) .
C10 C20 1.504(3) .
C11 C21 1.394(4) .
C11 C23 1.397(3) .
C11 C24 1.505(4) .
C14 C26 1.395(3) .
C19 C26 1.506(4) .
C21 C26 1.382(4) .
C100 C101 1.448(9) .
C101 C102 1.378(8) .
C101 C106 1.385(8) .
C102 C103 1.379(9) .
C103 C104 1.384(8) .
C104 C105 1.380(9) .
C105 C106 1.355(8) .
C200 C201 1.449(10) .
C201 C202 1.377(10) .
C201 C206 1.386(10) .
C202 C203 1.379(11) .
C203 C204 1.386(9) .
C204 C205 1.380(10) .
C205 C206 1.357(10) .
C300 C301 1.447(11) .
C301 C302 1.375(11) .
C301 C306 1.390(10) .
C302 C303 1.379(11) .
C303 C304 1.383(10) .
C304 C305 1.383(11) .
C305 C306 1.352(11) .
