Grafting of a new bis-silylamido aluminum species on silica: insight from solid-state NMR into interactions with the surface.
Vancompernolle, Tom; Merle, Nicolas; Capet, Frédéric; Del Rosal, Iker; Laurent, Maron; Delevoye, Laurent; Pourpoint, Frédérique; Gauvin, Régis M; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5243–5252; doi:10.1039/c9dt00845d

data_7049351
_publ_section_title
;
 Grafting of a new bis-silylamido aluminum species on silica: insight from
 solid-state NMR into interactions with the surface.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5243
_journal_page_last               5252
_journal_paper_doi               10.1039/c9dt00845d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C16 H44 Al Cl N2 O Si4'
_chemical_formula_sum            'C16 H44 Al Cl N2 O Si4'
_chemical_formula_weight         455.32
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-10 deposited with the CCDC.    2019-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                104.962(2)
_cell_angle_beta                 93.099(2)
_cell_angle_gamma                109.088(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3419(4)
_cell_length_b                   11.3931(5)
_cell_length_c                   15.5621(7)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.61
_cell_volume                     1334.69(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43905
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.474
_diffrn_reflns_theta_min         1.370
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0910 before and 0.0441 after correction. The Ratio of minimum to maximum transmission is 0.9471. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         8084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0294
_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/[\s^2^(Fo^2^)+(0.0356P)^2^+0.5193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6852
_reflns_number_total             8084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00845d3.cif
_cod_data_source_block           mo_tv155
_cod_depositor_comments          'Adding full bibliography for 7049351.cif.'
_cod_database_code               7049351
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H3AA)=Sof(H3AB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H1AA)=Sof(H1AB)=1-FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H1BC)=Sof(H1BD)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3BC,H3BD), C3(H3AA,H3AB), C2A(H2AA,H2AB), C2B(H2BA,H2BB),
 C1(H1BC,H1BD), C1(H1AA,H1AB)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C),
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              43386
_olex2_submission_special_instructions 'No special instructions were received'