#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:52:33 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195103 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/22/7042248.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_7042248
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         'C26 H33 Al N P'
_chemical_formula_sum            'C26 H33 Al N P'
_chemical_formula_weight         417.48
_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   geom
_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                96.545(3)
_cell_angle_beta                 99.302(3)
_cell_angle_gamma                109.982(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7257(15)
_cell_length_b                   10.3432(17)
_cell_length_c                   12.758(2)
_cell_measurement_reflns_used    1232
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.332
_cell_measurement_theta_min      3.582
_cell_volume                     1170.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Nonius Kappa'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24513
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.563
_diffrn_reflns_theta_min         1.645
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0853 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.8132.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         6532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0341
_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)+(0.0328P)²+0.6500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5753
_reflns_number_total             6532
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00318h2.cif
_cod_data_source_block           hz1301
_cod_depositor_comments
'Adding full bibliography for 7042248--7042253.cif.'
_cod_database_code               7042248
_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:
 C14(H14), C20(H20)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C16(H16), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
C1 C 0.48520(12) 0.28849(12) 0.14912(9) 0.0158(2) Uani 1 1 d .
H1 H 0.3967 0.3073 0.1281 0.019 Uiso 1 1 calc R
C2 C 0.70855(12) 0.32175(12) 0.28011(9) 0.0158(2) Uani 1 1 d .
H2 H 0.7725 0.3627 0.3493 0.019 Uiso 1 1 calc R
C3 C 0.57568(12) 0.34693(11) 0.25341(8) 0.01302(19) Uani 1 1 d .
C4 C 0.52481(13) 0.20341(12) 0.07678(9) 0.0181(2) Uani 1 1 d .
H4 H 0.4619 0.1627 0.0072 0.022 Uiso 1 1 calc R
C5 C 0.74859(13) 0.23767(13) 0.20690(9) 0.0183(2) Uani 1 1 d .
H5 H 0.8391 0.2216 0.2263 0.022 Uiso 1 1 calc R
C6 C 0.65588(14) 0.17739(12) 0.10553(9) 0.0188(2) Uani 1 1 d .
H6 H 0.6818 0.1186 0.0560 0.023 Uiso 1 1 calc R
C7 C 0.61007(13) 0.75566(12) 0.34113(9) 0.0182(2) Uani 1 1 d .
H7 H 0.5696 0.7569 0.4040 0.022 Uiso 1 1 calc R
C8 C 0.61149(12) 0.62937(11) 0.28902(8) 0.0133(2) Uani 1 1 d .
C9 C 0.67620(14) 0.63105(13) 0.19830(10) 0.0192(2) Uani 1 1 d .
H9 H 0.6799 0.5470 0.1625 0.023 Uiso 1 1 calc R
C10 C 0.72949(13) 0.87858(13) 0.21128(10) 0.0209(2) Uani 1 1 d .
H10 H 0.7683 0.9626 0.1842 0.025 Uiso 1 1 calc R
C11 C 0.66706(14) 0.87930(13) 0.30209(10) 0.0214(2) Uani 1 1 d .
H11 H 0.6633 0.9637 0.3373 0.026 Uiso 1 1 calc R
C12 C 0.73508(14) 0.75533(13) 0.16035(10) 0.0228(2) Uani 1 1 d .
H12 H 0.7793 0.7555 0.0992 0.027 Uiso 1 1 calc R
C13 C 0.75318(11) 0.66752(11) 0.73339(8) 0.01224(19) Uani 1 1 d .
C14 C 0.74266(14) 0.88488(12) 0.65412(10) 0.0192(2) Uani 1 1 d .
H14 H 0.6709 0.8100 0.5938 0.023 Uiso 1 1 calc R
C15 C 0.80197(12) 0.81443(12) 0.73969(9) 0.0145(2) Uani 1 1 d .
C16 C 0.92755(12) 0.70190(13) 0.90254(9) 0.0169(2) Uani 1 1 d .
H16 H 0.9711 0.6644 0.9576 0.020 Uiso 1 1 calc R
C17 C 0.81902(12) 0.61056(12) 0.81430(8) 0.0138(2) Uani 1 1 d .
C18 C 0.91085(12) 0.90051(12) 0.82965(9) 0.0170(2) Uani 1 1 d .
H18 H 0.9434 0.9992 0.8351 0.020 Uiso 1 1 calc R
C19 C 0.97254(13) 0.84575(13) 0.91103(9) 0.0184(2) Uani 1 1 d .
H19 H 1.0449 0.9062 0.9720 0.022 Uiso 1 1 calc R
C20 C 0.77963(12) 0.45404(12) 0.80864(9) 0.0160(2) Uani 1 1 d .
H20 H 0.6963 0.4049 0.7441 0.019 Uiso 1 1 calc R
C21 C 0.91425(14) 0.41422(13) 0.79198(11) 0.0227(2) Uani 1 1 d .
H21A H 0.9439 0.4425 0.7258 0.034 Uiso 1 1 calc GR
H21B H 0.8863 0.3128 0.7858 0.034 Uiso 1 1 calc GR
H21C H 0.9983 0.4620 0.8538 0.034 Uiso 1 1 calc GR
C22 C 0.72476(15) 0.40374(15) 0.90829(10) 0.0261(3) Uani 1 1 d .
H22A H 0.8062 0.4464 0.9724 0.039 Uiso 1 1 calc GR
H22B H 0.6932 0.3017 0.8982 0.039 Uiso 1 1 calc GR
H22C H 0.6399 0.4310 0.9179 0.039 Uiso 1 1 calc GR
C23 C 0.65871(15) 0.97393(14) 0.69768(12) 0.0266(3) Uani 1 1 d .
H23A H 0.5743 0.9146 0.7244 0.040 Uiso 1 1 calc GR
H23B H 0.6212 1.0155 0.6396 0.040 Uiso 1 1 calc GR
H23C H 0.7271 1.0484 0.7568 0.040 Uiso 1 1 calc GR
C24 C 0.86995(16) 0.97828(14) 0.60741(11) 0.0265(3) Uani 1 1 d .
H24A H 0.9375 1.0568 0.6639 0.040 Uiso 1 1 calc GR
H24B H 0.8274 1.0142 0.5475 0.040 Uiso 1 1 calc GR
H24C H 0.9259 0.9232 0.5811 0.040 Uiso 1 1 calc GR
C25 C 0.90211(12) 0.63012(13) 0.51939(9) 0.0185(2) Uani 1 1 d .
H25A H 0.8878 0.7101 0.4914 0.028 Uiso 1 1 calc GR
H25B H 0.9461 0.5844 0.4701 0.028 Uiso 1 1 calc GR
H25C H 0.9694 0.6628 0.5909 0.028 Uiso 1 1 calc GR
C26 C 0.68761(13) 0.29729(12) 0.52957(9) 0.0166(2) Uani 1 1 d .
H26A H 0.6771 0.2741 0.6010 0.025 Uiso 1 1 calc GR
H26B H 0.7770 0.2844 0.5118 0.025 Uiso 1 1 calc GR
H26C H 0.5989 0.2357 0.4753 0.025 Uiso 1 1 calc GR
N1 N 0.63602(10) 0.57619(9) 0.64247(7) 0.01160(17) Uani 1 1 d .
Al1 Al 0.70761(4) 0.49601(3) 0.53083(3) 0.01161(7) Uani 1 1 d .
P1 P 0.54469(3) 0.47297(3) 0.35068(2) 0.01069(7) 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'
N N 0.0061 0.0033 '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'
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
C4 C1 C3 120.35(10) . .
C5 C2 C3 121.14(10) . .
C1 C3 P1 124.19(8) . .
C2 C3 C1 118.25(10) . .
C2 C3 P1 117.03(8) . .
C1 C4 C6 120.53(10) . .
C6 C5 C2 119.87(11) . .
C5 C6 C4 119.80(11) . .
C11 C7 C8 121.04(11) . .
C7 C8 C9 118.39(10) . .
C7 C8 P1 118.23(8) . .
C9 C8 P1 123.12(9) . .
C12 C9 C8 120.42(11) . .
C12 C10 C11 120.00(11) . .
C10 C11 C7 119.69(11) . .
C10 C12 C9 120.43(11) . .
C15 C13 N1 119.32(9) . .
C17 C13 C15 120.10(10) . .
C17 C13 N1 120.58(10) . .
C15 C14 C23 112.48(10) . .
C15 C14 C24 111.37(10) . .
C23 C14 C24 108.72(10) . .
C13 C15 C14 123.80(10) . .
C18 C15 C13 118.43(10) . .
C18 C15 C14 117.77(10) . .
C19 C16 C17 121.35(10) . .
C13 C17 C20 122.84(9) . .
C16 C17 C13 118.88(10) . .
C16 C17 C20 118.27(10) . .
C19 C18 C15 121.85(11) . .
C16 C19 C18 119.32(10) . .
C17 C20 C21 110.26(9) . .
C17 C20 C22 112.55(10) . .
C22 C20 C21 110.78(10) . .
C13 N1 Al1 114.39(7) . .
C13 N1 P1 120.68(7) . 2_666
P1 N1 Al1 124.09(5) 2_666 .
C25 Al1 C26 117.76(5) . .
C25 Al1 P1 102.44(4) . .
C26 Al1 P1 100.47(4) . .
N1 Al1 C25 109.35(5) . .
N1 Al1 C26 115.62(5) . .
N1 Al1 P1 109.69(3) . .
C3 P1 C8 99.10(5) . .
C3 P1 Al1 108.05(4) . .
C8 P1 Al1 112.44(4) . .
N1 P1 C3 111.46(5) 2_666 .
N1 P1 C8 113.76(5) 2_666 .
N1 P1 Al1 111.29(3) 2_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C3 1.4088(15) .
C1 C4 1.3914(16) .
C2 C3 1.4007(15) .
C2 C5 1.3943(16) .
C3 P1 1.8305(11) .
C4 C6 1.3920(17) .
C5 C6 1.3890(16) .
C7 C8 1.4020(16) .
C7 C11 1.3931(16) .
C8 C9 1.4031(15) .
C8 P1 1.8424(11) .
C9 C12 1.3939(17) .
C10 C11 1.3927(18) .
C10 C12 1.3856(18) .
C13 C15 1.4169(15) .
C13 C17 1.4162(15) .
C13 N1 1.4572(13) .
C14 C15 1.5233(16) .
C14 C23 1.5388(18) .
C14 C24 1.5405(18) .
C15 C18 1.4005(15) .
C16 C17 1.4021(15) .
C16 C19 1.3856(17) .
C17 C20 1.5210(16) .
C18 C19 1.3870(17) .
C20 C21 1.5386(17) .
C20 C22 1.5336(17) .
C25 Al1 1.9662(12) .
C26 Al1 1.9952(12) .
N1 Al1 1.9097(10) .
N1 P1 1.6746(10) 2_666
Al1 P1 2.5080(5) .
P1 N1 1.6745(10) 2_666
