#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:52:33 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195103 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/22/7042253.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_7042253
loop_
_publ_author_name
'Zijlstra, Harmen S.'
'Pahl, Jürgen'
'Penafiel, Johanne'
'Harder, Sjoerd'
_publ_section_title
;
 "Masked" Lewis-acidity of an aluminum α-phosphinoamide
 complex.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3601
_journal_page_last               3610
_journal_paper_doi               10.1039/c7dt00318h
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C54 H66 Al2 N2 O4 P2, C6 H6'
_chemical_formula_sum            'C60 H72 Al2 N2 O4 P2'
_chemical_formula_weight         1001.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-01-19 deposited with the CCDC.
2017-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.651(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0550(3)
_cell_length_b                   12.3310(7)
_cell_length_c                   19.9820(9)
_cell_measurement_reflns_used    1427
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.013
_cell_measurement_theta_min      3.259
_cell_volume                     2778.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Nonius Kappa'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            93690
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.502
_diffrn_reflns_theta_min         2.924
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         8463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0372
_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)+(0.0516P)²+1.2502P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6890
_reflns_number_total             8463
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00318h2.cif
_cod_data_source_block           pj1
_cod_depositor_comments
'Adding full bibliography for 7042248--7042253.cif.'
_cod_original_cell_volume        2778.4(2)
_cod_database_code               7042253
_shelx_shelxl_version_number     2014/7
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29), C30(H30)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
P1 P 0.58925(2) 0.69969(2) 0.69108(2) 0.01408(7) Uani 1 1 d .
Al1 Al 0.37320(3) 0.57552(3) 0.50541(2) 0.01492(8) Uani 1 1 d .
O1 O 0.52586(7) 0.60211(7) 0.54346(5) 0.01593(16) Uani 1 1 d .
O2 O 0.68424(7) 0.49588(7) 0.59384(5) 0.01852(17) Uani 1 1 d .
N1 N 0.68024(8) 0.61081(8) 0.68096(6) 0.01361(18) Uani 1 1 d .
C1 C 0.79788(10) 0.57615(9) 0.75100(7) 0.0141(2) Uani 1 1 d .
C2 C 0.80790(10) 0.49236(9) 0.80292(7) 0.0173(2) Uani 1 1 d .
C3 C 0.92061(12) 0.46919(11) 0.87539(8) 0.0244(3) Uani 1 1 d .
H3 H 0.9295 0.4149 0.9110 0.029 Uiso 1 1 calc R
C4 C 1.01968(12) 0.52588(12) 0.89517(8) 0.0269(3) Uani 1 1 d .
H4 H 1.0936 0.5113 0.9448 0.032 Uiso 1 1 calc R
C5 C 1.00858(11) 0.60405(11) 0.84127(8) 0.0232(3) Uani 1 1 d .
H5 H 1.0759 0.6397 0.8541 0.028 Uiso 1 1 calc R
C6 C 0.89762(10) 0.63058(10) 0.76759(7) 0.0170(2) Uani 1 1 d .
C7 C 0.70194(12) 0.42442(10) 0.77977(8) 0.0220(2) Uani 1 1 d .
H7 H 0.6302 0.4676 0.7423 0.026 Uiso 1 1 calc R
C8 C 0.70485(15) 0.39114(14) 0.85477(10) 0.0341(3) Uani 1 1 d .
H8A H 0.7693 0.3416 0.8891 0.051 Uiso 1 1 calc GR
H8B H 0.6314 0.3565 0.8355 0.051 Uiso 1 1 calc GR
H8C H 0.7157 0.4544 0.8867 0.051 Uiso 1 1 calc GR
C9 C 0.69419(15) 0.32333(12) 0.73190(10) 0.0331(3) Uani 1 1 d .
H9A H 0.6909 0.3450 0.6844 0.050 Uiso 1 1 calc GR
H9B H 0.6240 0.2830 0.7135 0.050 Uiso 1 1 calc GR
H9C H 0.7628 0.2787 0.7678 0.050 Uiso 1 1 calc GR
C10 C 0.89171(11) 0.71237(11) 0.70846(8) 0.0217(2) Uani 1 1 d .
H10 H 0.8083 0.7210 0.6608 0.026 Uiso 1 1 calc R
C11 C 0.93926(14) 0.82390(13) 0.74867(10) 0.0339(3) Uani 1 1 d .
H11A H 0.8959 0.8501 0.7685 0.051 Uiso 1 1 calc GR
H11B H 0.9299 0.8736 0.7081 0.051 Uiso 1 1 calc GR
H11C H 1.0218 0.8180 0.7946 0.051 Uiso 1 1 calc GR
C12 C 0.95847(15) 0.66814(17) 0.67558(10) 0.0401(4) Uani 1 1 d .
H12A H 1.0393 0.6537 0.7216 0.060 Uiso 1 1 calc GR
H12B H 0.9564 0.7207 0.6393 0.060 Uiso 1 1 calc GR
H12C H 0.9215 0.6023 0.6452 0.060 Uiso 1 1 calc GR
C13 C 0.65861(10) 0.69317(10) 0.80257(7) 0.0168(2) Uani 1 1 d .
C14 C 0.58378(12) 0.65744(11) 0.82233(8) 0.0225(2) Uani 1 1 d .
H14 H 0.5066 0.6364 0.7798 0.027 Uiso 1 1 calc R
C15 C 0.62341(14) 0.65292(13) 0.90504(9) 0.0295(3) Uani 1 1 d .
H15 H 0.5729 0.6291 0.9175 0.035 Uiso 1 1 calc R
C16 C 0.73803(14) 0.68391(13) 0.96836(8) 0.0293(3) Uani 1 1 d .
H16 H 0.7647 0.6808 1.0235 0.035 Uiso 1 1 calc R
C17 C 0.81382(12) 0.71975(12) 0.94976(8) 0.0260(3) Uani 1 1 d .
H17 H 0.8910 0.7402 0.9926 0.031 Uiso 1 1 calc R
C18 C 0.77455(11) 0.72507(11) 0.86749(8) 0.0203(2) Uani 1 1 d .
H18 H 0.8252 0.7498 0.8554 0.024 Uiso 1 1 calc R
C19 C 0.63230(10) 0.83450(10) 0.67917(7) 0.0164(2) Uani 1 1 d .
C20 C 0.62372(11) 0.85839(10) 0.60703(8) 0.0211(2) Uani 1 1 d .
H20 H 0.6033 0.8040 0.5684 0.025 Uiso 1 1 calc R
C21 C 0.64543(13) 0.96280(11) 0.59294(9) 0.0273(3) Uani 1 1 d .
H21 H 0.6417 0.9773 0.5457 0.033 Uiso 1 1 calc R
C22 C 0.67267(13) 1.04559(11) 0.64885(9) 0.0280(3) Uani 1 1 d .
H22 H 0.6880 1.1152 0.6396 0.034 Uiso 1 1 calc R
C23 C 0.67680(13) 1.02354(11) 0.71846(9) 0.0261(3) Uani 1 1 d .
H23 H 0.6931 1.0792 0.7553 0.031 Uiso 1 1 calc R
C24 C 0.65688(12) 0.91916(10) 0.73398(8) 0.0212(2) Uani 1 1 d .
H24 H 0.6599 0.9056 0.7810 0.025 Uiso 1 1 calc R
C25 C 0.62866(9) 0.56691(9) 0.60419(7) 0.0138(2) Uani 1 1 d .
C26 C 0.36758(13) 0.47426(12) 0.57815(9) 0.0279(3) Uani 1 1 d .
H26A H 0.4233 0.4166 0.5941 0.042 Uiso 1 1 calc GR
H26B H 0.2891 0.4447 0.5490 0.042 Uiso 1 1 calc GR
H26C H 0.3876 0.5117 0.6271 0.042 Uiso 1 1 calc GR
C27 C 0.29101(12) 0.71509(11) 0.47067(8) 0.0242(3) Uani 1 1 d .
H27A H 0.3479 0.7726 0.4900 0.036 Uiso 1 1 calc GR
H27B H 0.2485 0.7238 0.4941 0.036 Uiso 1 1 calc GR
H27C H 0.2363 0.7175 0.4109 0.036 Uiso 1 1 calc GR
C28 C 1.05050(17) 0.50055(18) 0.58389(11) 0.0480(5) Uani 1 1 d .
H28 H 1.0841 0.5015 0.6405 0.058 Uiso 1 1 calc R
C29 C 0.96647(18) 0.4251(2) 0.53284(13) 0.0601(6) Uani 1 1 d .
H29 H 0.9439 0.3736 0.5549 0.072 Uiso 1 1 calc R
C30 C 0.9149(2) 0.4253(2) 0.44861(13) 0.0621(6) Uani 1 1 d .
H30 H 0.8565 0.3747 0.4138 0.075 Uiso 1 1 calc R
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'
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_
_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
N1 P1 C13 102.39(5) . .
N1 P1 C19 103.17(5) . .
C13 P1 C19 102.79(5) . .
O1 Al1 O2 100.56(4) . 3_666
O1 Al1 C26 111.35(5) . .
O1 Al1 C27 106.73(5) . .
O2 Al1 C26 107.86(6) 3_666 .
O2 Al1 C27 104.48(5) 3_666 .
C26 Al1 C27 123.31(6) . .
C25 O1 Al1 135.25(8) . .
C25 O2 Al1 125.68(7) . 3_666
C1 N1 P1 123.49(7) . .
C25 N1 P1 115.93(7) . .
C25 N1 C1 120.25(9) . .
C2 C1 N1 118.71(10) . .
C6 C1 N1 119.24(10) . .
C6 C1 C2 121.96(10) . .
C1 C2 C7 122.03(10) . .
C3 C2 C1 117.78(11) . .
C3 C2 C7 120.11(11) . .
C2 C3 H3 119.5 . .
C4 C3 C2 121.10(12) . .
C4 C3 H3 119.5 . .
C3 C4 H4 119.9 . .
C5 C4 C3 120.10(12) . .
C5 C4 H4 119.9 . .
C4 C5 H5 119.4 . .
C4 C5 C6 121.20(12) . .
C6 C5 H5 119.4 . .
C1 C6 C10 123.44(10) . .
C5 C6 C1 117.68(11) . .
C5 C6 C10 118.84(11) . .
C2 C7 H7 107.9 . .
C2 C7 C8 113.65(12) . .
C2 C7 C9 109.23(11) . .
C8 C7 H7 107.9 . .
C8 C7 C9 110.05(12) . .
C9 C7 H7 107.9 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C6 C10 H10 107.8 . .
C6 C10 C11 112.63(11) . .
C6 C10 C12 109.54(12) . .
C11 C10 H10 107.8 . .
C11 C10 C12 110.97(13) . .
C12 C10 H10 107.8 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11B 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12B 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C14 C13 P1 114.55(9) . .
C14 C13 C18 118.80(11) . .
C18 C13 P1 126.57(9) . .
C13 C14 H14 119.6 . .
C15 C14 C13 120.79(12) . .
C15 C14 H14 119.6 . .
C14 C15 H15 120.1 . .
C16 C15 C14 119.78(13) . .
C16 C15 H15 120.1 . .
C15 C16 H16 119.9 . .
C15 C16 C17 120.19(12) . .
C17 C16 H16 119.9 . .
C16 C17 H17 119.9 . .
C18 C17 C16 120.26(13) . .
C18 C17 H17 119.9 . .
C13 C18 H18 119.9 . .
C17 C18 C13 120.19(12) . .
C17 C18 H18 119.9 . .
C20 C19 P1 119.40(9) . .
C24 C19 P1 121.44(9) . .
C24 C19 C20 118.49(11) . .
C19 C20 H20 119.8 . .
C21 C20 C19 120.50(12) . .
C21 C20 H20 119.8 . .
C20 C21 H21 119.8 . .
C22 C21 C20 120.44(12) . .
C22 C21 H21 119.8 . .
C21 C22 H22 120.3 . .
C23 C22 C21 119.36(13) . .
C23 C22 H22 120.3 . .
C22 C23 H23 119.6 . .
C22 C23 C24 120.84(13) . .
C24 C23 H23 119.6 . .
C19 C24 H24 119.9 . .
C23 C24 C19 120.30(12) . .
C23 C24 H24 119.9 . .
O1 C25 N1 118.21(10) . .
O2 C25 O1 122.18(10) . .
O2 C25 N1 119.56(10) . .
Al1 C26 H26A 109.5 . .
Al1 C26 H26B 109.5 . .
Al1 C26 H26C 109.5 . .
H26A C26 H26B 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
Al1 C27 H27A 109.5 . .
Al1 C27 H27B 109.5 . .
Al1 C27 H27C 109.5 . .
H27A C27 H27B 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C29 C28 H28 120.2 . .
C29 C28 C30 119.68(18) . 3_766
C30 C28 H28 120.2 3_766 .
C28 C29 H29 120.0 . .
C28 C29 C30 120.1(2) . .
C30 C29 H29 120.0 . .
C28 C30 C29 120.2(2) 3_766 .
C28 C30 H30 119.9 3_766 .
C29 C30 H30 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 N1 1.7849(10) .
P1 C13 1.8241(12) .
P1 C19 1.8325(12) .
Al1 O1 1.8279(9) .
Al1 O2 1.8571(9) 3_666
Al1 C26 1.9532(14) .
Al1 C27 1.9547(13) .
O1 C25 1.2866(13) .
O2 Al1 1.8571(9) 3_666
O2 C25 1.2701(14) .
N1 C1 1.4535(14) .
N1 C25 1.3580(14) .
C1 C2 1.4104(16) .
C1 C6 1.4038(16) .
C2 C3 1.3962(17) .
C2 C7 1.5203(17) .
C3 H3 0.9300 .
C3 C4 1.388(2) .
C4 H4 0.9300 .
C4 C5 1.383(2) .
C5 H5 0.9300 .
C5 C6 1.4020(16) .
C6 C10 1.5175(17) .
C7 H7 0.9800 .
C7 C8 1.531(2) .
C7 C9 1.535(2) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10 0.9800 .
C10 C11 1.531(2) .
C10 C12 1.531(2) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C14 1.3971(17) .
C13 C18 1.4033(17) .
C14 H14 0.9300 .
C14 C15 1.3949(18) .
C15 H15 0.9300 .
C15 C16 1.382(2) .
C16 H16 0.9300 .
C16 C17 1.393(2) .
C17 H17 0.9300 .
C17 C18 1.3885(17) .
C18 H18 0.9300 .
C19 C20 1.4041(17) .
C19 C24 1.3989(17) .
C20 H20 0.9300 .
C20 C21 1.3902(19) .
C21 H21 0.9300 .
C21 C22 1.388(2) .
C22 H22 0.9300 .
C22 C23 1.384(2) .
C23 H23 0.9300 .
C23 C24 1.3909(18) .
C24 H24 0.9300 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
C28 H28 0.9300 .
C28 C29 1.365(3) .
C28 C30 1.368(3) 3_766
C29 H29 0.9300 .
C29 C30 1.379(3) .
C30 C28 1.368(3) 3_766
C30 H30 0.9300 .
