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#$Date: 2023-08-10 01:57:07 +0300 (Thu, 10 Aug 2023) $
#$Revision: 285608 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/37/7713708.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_7713708
loop_
_publ_author_name
'Vrána, Jan'
'Ruzickova, Zdenka'
'R°užička, Aleš'
'Dostál, Libor'
_publ_section_title
;
 Synthesis and reactivity of alkali metal aluminates bearing
 bis(organoamido)phosphane ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01859H
_journal_year                    2023
_chemical_formula_moiety         'C36 H66 Al2 Li2 N4 O2 P2'
_chemical_formula_sum            'C36 H66 Al2 Li2 N4 O2 P2'
_chemical_formula_weight         716.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-07-25 deposited with the CCDC.	2023-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                105.389(4)
_cell_angle_beta                 104.811(3)
_cell_angle_gamma                110.097(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3410(4)
_cell_length_b                   10.4790(4)
_cell_length_c                   11.8430(4)
_cell_measurement_reflns_used    22689
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1073.37(9)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22689
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         1.931
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0305
_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)+(0.0289P)²+0.4446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4275
_reflns_number_total             4901
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt01859h2.cif
_cod_data_source_block           ld141123Al1
_cod_original_cell_volume        1073.37(8)
_cod_database_code               7713708
_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.
;
_shelxl_version_number           2013-4
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
P1 P 0.55169(3) 0.42272(3) 0.17999(3) 0.01698(8) Uani 1 1 d . . . . .
Al1 Al 0.51443(4) 0.30511(4) 0.34638(3) 0.01857(9) Uani 1 1 d . . . . .
N1 N 0.41442(10) 0.38379(10) 0.24364(9) 0.01783(19) Uani 1 1 d . . . . .
O1 O 0.36065(11) 0.71920(11) 0.31062(9) 0.0289(2) Uani 1 1 d . . . . .
N2 N 0.64598(11) 0.35604(11) 0.26865(9) 0.01820(19) Uani 1 1 d . . . . .
C1 C 0.65482(13) 0.62546(13) 0.27159(11) 0.0189(2) Uani 1 1 d . . . . .
C3 C 0.80481(15) 0.84107(14) 0.46747(12) 0.0290(3) Uani 1 1 d . . . . .
H3 H 0.8539 0.8821 0.5552 0.035 Uiso 1 1 d R U . . .
C6 C 0.65651(14) 0.71881(14) 0.20648(12) 0.0236(2) Uani 1 1 d . . . . .
H6 H 0.6067 0.6787 0.1189 0.028 Uiso 1 1 d R U . . .
C7 C 0.25724(13) 0.28699(14) 0.14974(11) 0.0234(2) Uani 1 1 d . . . . .
C2 C 0.73188(14) 0.68915(13) 0.40324(12) 0.0240(3) Uani 1 1 d . . . . .
H2 H 0.7341 0.6288 0.4482 0.029 Uiso 1 1 d R U . . .
C5 C 0.73160(16) 0.87115(14) 0.27112(13) 0.0297(3) Uani 1 1 d . . . . .
H5 H 0.7327 0.9320 0.2264 0.036 Uiso 1 1 d R U . . .
C9 C 0.16111(15) 0.25139(17) 0.22649(14) 0.0350(3) Uani 1 1 d . . . . .
H9A H 0.1895 0.1940 0.2700 0.042 Uiso 1 1 d R U . . .
H9B H 0.0581 0.1963 0.1705 0.042 Uiso 1 1 d R U . . .
H9C H 0.1754 0.3416 0.2872 0.042 Uiso 1 1 d R U . . .
C11 C 0.76122(13) 0.31812(13) 0.24075(12) 0.0219(2) Uani 1 1 d . . . . .
C13 C 0.83743(15) 0.28566(16) 0.35104(13) 0.0297(3) Uani 1 1 d . . . . .
H13A H 0.8851 0.3729 0.4275 0.036 Uiso 1 1 d R U . . .
H13B H 0.9107 0.2558 0.3338 0.036 Uiso 1 1 d R U . . .
H13C H 0.7644 0.2080 0.3611 0.036 Uiso 1 1 d R U . . .
C15 C 0.34986(17) 0.76767(17) 0.20701(14) 0.0333(3) Uani 1 1 d . . . . .
H15A H 0.3566 0.7007 0.1369 0.040 Uiso 1 1 d R U . . .
H15B H 0.4281 0.8660 0.2336 0.040 Uiso 1 1 d R U . . .
C12 C 0.87630(16) 0.44595(17) 0.22819(17) 0.0374(3) Uani 1 1 d . . . . .
H12A H 0.8282 0.4669 0.1595 0.045 Uiso 1 1 d R U . . .
H12B H 0.9518 0.4196 0.2117 0.045 Uiso 1 1 d R U . . .
H12C H 0.9212 0.5317 0.3056 0.045 Uiso 1 1 d R U . . .
C8 C 0.24134(15) 0.14260(14) 0.05867(13) 0.0303(3) Uani 1 1 d . . . . .
H8A H 0.3048 0.1643 0.0129 0.036 Uiso 1 1 d R U . . .
H8B H 0.1396 0.0846 0.0000 0.036 Uiso 1 1 d R U . . .
H8C H 0.2695 0.0884 0.1061 0.036 Uiso 1 1 d R U . . .
C4 C 0.80464(16) 0.93216(14) 0.40131(13) 0.0296(3) Uani 1 1 d . . . . .
H4 H 0.8535 1.0341 0.4444 0.035 Uiso 1 1 d R U . . .
C14 C 0.69094(18) 0.18053(17) 0.11831(13) 0.0356(3) Uani 1 1 d . . . . .
H14A H 0.6213 0.0993 0.1274 0.043 Uiso 1 1 d R U . . .
H14B H 0.7676 0.1567 0.1013 0.043 Uiso 1 1 d R U . . .
H14C H 0.6399 0.1994 0.0493 0.043 Uiso 1 1 d R U . . .
C10 C 0.20390(16) 0.36788(16) 0.07244(13) 0.0332(3) Uani 1 1 d . . . . .
H10A H 0.2046 0.4537 0.1282 0.040 Uiso 1 1 d R U . . .
H10B H 0.1044 0.3036 0.0111 0.040 Uiso 1 1 d R U . . .
H10C H 0.2690 0.3973 0.0296 0.040 Uiso 1 1 d R U . . .
C17 C 0.18764(17) 0.82255(16) 0.29758(15) 0.0354(3) Uani 1 1 d . . . . .
H17A H 0.2275 0.9292 0.3318 0.043 Uiso 1 1 d R U . . .
H17B H 0.0850 0.7802 0.2905 0.043 Uiso 1 1 d R U . . .
C16 C 0.19820(18) 0.76612(18) 0.16983(15) 0.0381(3) Uani 1 1 d . . . . .
H16A H 0.1198 0.6673 0.1168 0.046 Uiso 1 1 d R U . . .
H16B H 0.1930 0.8311 0.1256 0.046 Uiso 1 1 d R U . . .
C18 C 0.28109(19) 0.77269(19) 0.38057(14) 0.0391(3) Uani 1 1 d . . . . .
H18A H 0.3506 0.8543 0.4602 0.047 Uiso 1 1 d R U . . .
H18B H 0.2175 0.6947 0.3986 0.047 Uiso 1 1 d R U . . .
Li1 Li 0.4408(2) 0.5872(2) 0.3512(2) 0.0253(4) Uani 1 1 d . . . . .
H1A H 0.436(2) 0.1449(17) 0.3300(17) 0.044(5) Uani 1 1 d . . . . .
H1B H 0.5753(18) 0.3999(18) 0.4933(15) 0.040(5) 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 0.0033 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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.186
0 0 1 0.165
0 -1 0 0.114
0 1 0 0.095
1 -1 0 0.087
-1 1 0 0.149
-1 0 0 0.167
1 0 0 0.088
1 0 -1 0.226
-1 0 1 0.247
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
N2 P1 N1 91.25(5) . . ?
N2 P1 C1 102.99(5) . . ?
N1 P1 C1 98.78(5) . . ?
N2 P1 Al1 44.16(3) . . ?
N1 P1 Al1 47.10(3) . . ?
C1 P1 Al1 105.99(4) . . ?
N2 P1 Li1 105.29(5) . . ?
N1 P1 Li1 41.29(5) . . ?
C1 P1 Li1 57.99(6) . . ?
Al1 P1 Li1 70.88(4) . . ?
N2 Al1 N1 81.71(4) . . ?
N2 Al1 P1 39.95(3) . . ?
N1 Al1 P1 41.76(3) . . ?
N2 Al1 H1A 119.8(7) . . ?
N1 Al1 H1A 120.2(7) . . ?
P1 Al1 H1A 131.2(7) . . ?
N2 Al1 H1B 115.6(6) . . ?
N1 Al1 H1B 112.8(6) . . ?
P1 Al1 H1B 123.0(6) . . ?
H1A Al1 H1B 105.8(9) . . ?
C7 N1 P1 116.03(8) . . ?
C7 N1 Al1 119.31(8) . . ?
P1 N1 Al1 91.14(4) . . ?
C7 N1 Li1 112.06(9) . . ?
P1 N1 Li1 104.52(8) . . ?
Al1 N1 Li1 111.31(7) . . ?
C15 O1 C18 107.82(10) . . ?
C15 O1 Li1 130.69(10) . . ?
C18 O1 Li1 121.11(11) . . ?
C11 N2 P1 122.21(8) . . ?
C11 N2 Al1 138.75(8) . . ?
P1 N2 Al1 95.90(5) . . ?
C6 C1 C2 118.29(11) . . ?
C6 C1 P1 118.75(9) . . ?
C2 C1 P1 122.97(9) . . ?
C6 C1 Li1 109.18(9) . . ?
C2 C1 Li1 78.05(9) . . ?
P1 C1 Li1 84.17(6) . . ?
C2 C3 C4 120.17(12) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 119.9 . . ?
C5 C6 C1 120.74(11) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.7 . . ?
N1 C7 C10 110.48(10) . . ?
N1 C7 C9 106.66(10) . . ?
C10 C7 C9 109.51(11) . . ?
N1 C7 C8 112.14(10) . . ?
C10 C7 C8 108.89(11) . . ?
C9 C7 C8 109.11(11) . . ?
C3 C2 C1 120.75(11) . . ?
C3 C2 Li1 111.25(10) . . ?
C1 C2 Li1 70.97(8) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
Li1 C2 H2 87.8 . . ?
C4 C5 C6 120.20(12) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 119.8 . . ?
C7 C9 H9A 109.6 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.3 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C11 C12 110.87(10) . . ?
N2 C11 C13 107.32(10) . . ?
C12 C11 C13 109.53(11) . . ?
N2 C11 C14 110.32(10) . . ?
C12 C11 C14 109.61(12) . . ?
C13 C11 C14 109.14(11) . . ?
C11 C13 H13A 109.4 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C15 C16 104.09(11) . . ?
O1 C15 H15A 110.9 . . ?
C16 C15 H15A 110.8 . . ?
O1 C15 H15B 111.0 . . ?
C16 C15 H15B 111.0 . . ?
H15A C15 H15B 109.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.4 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C4 C3 119.83(12) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.2 . . ?
C11 C14 H14A 109.6 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.4 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C10 H10A 109.4 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.6 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C17 C18 104.20(11) . . ?
C16 C17 H17A 111.0 . . ?
C18 C17 H17A 110.8 . . ?
C16 C17 H17B 110.9 . . ?
C18 C17 H17B 111.0 . . ?
H17A C17 H17B 108.9 . . ?
C15 C16 C17 102.18(12) . . ?
C15 C16 H16A 111.4 . . ?
C17 C16 H16A 111.4 . . ?
C15 C16 H16B 111.3 . . ?
C17 C16 H16B 111.2 . . ?
H16A C16 H16B 109.2 . . ?
O1 C18 C17 106.83(12) . . ?
O1 C18 H18A 110.5 . . ?
C17 C18 H18A 110.4 . . ?
O1 C18 H18B 110.3 . . ?
C17 C18 H18B 110.2 . . ?
H18A C18 H18B 108.6 . . ?
O1 Li1 N1 132.52(12) . . ?
O1 Li1 C1 105.07(10) . . ?
N1 Li1 C1 71.71(7) . . ?
O1 Li1 C2 113.17(10) . . ?
N1 Li1 C2 88.39(8) . . ?
C1 Li1 C2 30.99(4) . . ?
O1 Li1 P1 122.70(9) . . ?
N1 Li1 P1 34.19(4) . . ?
C1 Li1 P1 37.84(4) . . ?
C2 Li1 P1 60.42(5) . . ?
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
P1 N2 1.6958(10) . ?
P1 N1 1.7499(10) . ?
P1 C1 1.8591(12) . ?
P1 Al1 2.6271(5) . ?
P1 Li1 3.015(2) . ?
Al1 N2 1.8398(10) . ?
Al1 N1 1.9248(10) . ?
Al1 H1A 1.525(15) . ?
Al1 H1B 1.583(16) . ?
N1 C7 1.5006(15) . ?
N1 Li1 2.055(2) . ?
O1 C15 1.4408(16) . ?
O1 C18 1.4478(16) . ?
O1 Li1 1.941(2) . ?
N2 C11 1.4642(15) . ?
C1 C6 1.3954(16) . ?
C1 C2 1.3995(17) . ?
C1 Li1 2.570(2) . ?
C3 C2 1.3859(17) . ?
C3 C4 1.3865(19) . ?
C3 H3 0.9300 . ?
C6 C5 1.3904(18) . ?
C6 H6 0.9300 . ?
C7 C10 1.5283(18) . ?
C7 C9 1.5299(18) . ?
C7 C8 1.5336(17) . ?
C2 Li1 2.659(3) . ?
C2 H2 0.9300 . ?
C5 C4 1.3806(19) . ?
C5 H5 0.9299 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C11 C12 1.5276(18) . ?
C11 C13 1.5286(17) . ?
C11 C14 1.5301(18) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9601 . ?
C13 H13C 0.9600 . ?
C15 C16 1.510(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9599 . ?
C4 H4 0.9300 . ?
C14 H14A 0.9599 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9601 . ?
C10 H10A 0.9601 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9599 . ?
C17 C16 1.518(2) . ?
C17 C18 1.519(2) . ?
C17 H17A 0.9701 . ?
C17 H17B 0.9699 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
