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_7228788
_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         'C38 H53 Al N2 O'
_chemical_formula_sum            'C38 H53 Al N2 O'
_chemical_formula_weight         580.80
_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   mixed
_audit_creation_date             2016-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-05-05 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.781(2)
_cell_angle_beta                 94.755(2)
_cell_angle_gamma                108.004(2)
_cell_formula_units_Z            4
_cell_length_a                   12.120(3)
_cell_length_b                   14.739(3)
_cell_length_c                   22.976(4)
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      23.79
_cell_measurement_theta_min      2.18
_cell_volume                     3886.6(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_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  0.0766
_diffrn_reflns_av_unetI/netI     0.1014
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.417
_diffrn_reflns_theta_min         1.454
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0732 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.8975.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.993
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         19018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0960P)^2^+0.4942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.2030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11196
_reflns_number_total             19018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra06526d1.cif
_cod_data_source_block           2016_08_16_at266_nacalomes_0ma_a_sq
_cod_original_cell_volume        3886.5(13)
_cod_database_code               7228788
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.965
_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:
 C50(H50), C53(H53), C62(H62), C65(H65), C12(H12), C15(H15), C24(H24), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C46(H46), C47(H47), C48(H48), C58(H58), C59(H59), C60(H60),
 C70(H70), C72(H72), C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21),
 C22(H22), C32(H32), C34(H34)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C74(H74A,H74B,H74C),
 C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C),
 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), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              62451
_shelx_fab_checksum              27
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'