Reaction of sterically encumbered phenols, TEMPO-H, and organocarbonyl insertion reactions with L-AlH2 (L = HC(MeCNDipp)2, Dipp = 2,6-diisopropylphenyl)
Keyes, Lauren K.; Todd, Angela D. K.; Giffin, Nick A.; Veinot, Alex J.; Hendsbee, Arthur D.; Robertson, Katherine N.; Geier, Stephen J.; Masuda, Jason D.; RSC Adv. 7 (2017) 37315–; doi:10.1039/C7RA06526D

data_7228789
_publ_section_title
;
 Reaction of sterically encumbered phenols, TEMPO-H, and organocarbonyl
 insertion reactions with L-AlH2 (L = HC(MeCNDipp)2, Dipp =
 2,6-diisopropylphenyl)
;
_journal_issue                   59
_journal_name_full               'RSC Adv.'
_journal_page_first              37315
_journal_paper_doi               10.1039/C7RA06526D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         '2(C41 H59 Al N2 O), C5 H11'
_chemical_formula_sum            'C87 H129 Al2 N4 O2'
_chemical_formula_weight         1316.89
_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   mixed
_audit_creation_date             2016-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-05-05 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.731(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5098(16)
_cell_length_b                   15.1447(19)
_cell_length_c                   22.230(3)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.19
_cell_volume                     4073.2(9)
_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      99.97
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.947
_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  0.0839
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49947
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.190
_diffrn_reflns_theta_min         2.154
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1325 before and 0.0867 after correction.
The Ratio of minimum to maximum transmission is 0.7027.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_description       block
_exptl_crystal_F_000             1442
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         10430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+1.6935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7523
_reflns_number_total             10430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra06526d1.cif
_cod_data_source_block           lk03_0m_a
_cod_database_code               7228789
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C39B)=Sof(H39B)=Sof(C40B)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41B)=
 Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(1)
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=FVAR(1)
 Fixed Sof: C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C36(H36), C39(H39), C39B(H39B)
3.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B)
3.c Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C40B(H40D,H40E,H40F), C41B(H41D,H41E,H41F)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34)
3.e Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              98849
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'