"Masked" Lewis-acidity of an aluminum α-phosphinoamide complex.
Zijlstra, Harmen S.; Pahl, Jürgen; Penafiel, Johanne; Harder, Sjoerd; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3601–3610; doi:10.1039/c7dt00318h

data_7042250
_publ_section_title
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 &quot;Masked&quot; Lewis-acidity of an aluminum \a-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         '2(C30 H41 Al N P S)'
_chemical_formula_sum            'C60 H82 Al2 N2 P2 S2'
_chemical_formula_weight         1011.29
_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             2017-01-19
_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                88.25(2)
_cell_angle_beta                 89.542(16)
_cell_angle_gamma                80.584(16)
_cell_formula_units_Z            2
_cell_length_a                   9.296(2)
_cell_length_b                   16.751(3)
_cell_length_c                   18.941(5)
_cell_measurement_reflns_used    2196
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.176
_cell_measurement_theta_min      2.959
_cell_volume                     2908.3(11)
_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      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa Nonius'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1416
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63838
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.565
_diffrn_reflns_theta_min         2.711
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0959 before and 0.0787 after correction.
The Ratio of minimum to maximum transmission is 0.8131.
The \l/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    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         12047
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+6.8927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7292
_reflns_number_total             12047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00318h2.cif
_cod_data_source_block           hz1408_last_sx
_cod_depositor_comments
'Adding full bibliography for 7042248--7042253.cif.'
_cod_database_code               7042250
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 S1A, S1B, C30B, C30A, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H29C)=Sof(H29D)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(S1B)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(S1A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C28(H28), C37(H37), C40(H40), C58(H58)
4.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C29(H29A,H29B), C29(H29C,H29D), C57(H57A,H57B), C59(H59A,H59B)
4.c Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C60(H60A,H60B,H60C)
4.d 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), C33(H33), C34(H34), C35(H35),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54)
4.e Idealised Me refined as rotating group:
 C30A(H30A,H30B,H30C), C30B(H30D,H30E,H30F)
;
_olex2_submission_special_instructions 'No special instructions were received'