Unveiling the Takai Olefination Reagent via Tris( tert-butoxy)siloxy Variants.
Werner, Daniel; Anwander, Reiner; Journal of the American Chemical Society 140 (2018) 14334–14341; doi:10.1021/jacs.8b08739

data_4133167
_publ_section_title
;
 Unveiling the Takai Olefination Reagent via Tris( tert-butoxy)siloxy
 Variants.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14334
_journal_page_last               14341
_journal_paper_doi               10.1021/jacs.8b08739
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C49 H109 Cr2 I2 O16 Si4, C3 H7'
_chemical_formula_sum            'C52 H116 Cr2 I2 O16 Si4'
_chemical_formula_weight         1467.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                94.5434(14)
_cell_angle_beta                 107.6252(14)
_cell_angle_gamma                93.1097(14)
_cell_formula_units_Z            2
_cell_length_a                   13.6739(4)
_cell_length_b                   14.7859(4)
_cell_length_c                   19.0519(5)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.334
_cell_measurement_theta_min      2.748
_cell_volume                     3647.15(18)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            117347
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0507 before and 0.0421 after correction. The Ratio of minimum to maximum transmission is 0.9240. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.013
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         18203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+5.7736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                15509
_reflns_number_total             18203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b08739_si_006.cif
_cod_data_source_block           5b
_cod_original_cell_volume        3647.15(17)
_cod_database_code               4133167
_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.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C100(H10A,H10B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C29(H29A,H29B,
 H29C), C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C16(H16A,
 H16B,H16C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C),
 C5(H5A,H5B,H5C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C),
  C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C7(H7A,H7B,H7C), C23(H23A,H23B,
 H23C), C21(H21A,H21B,H21C), C40(H40A,H40B,H40C), C82(H82A,H82B,H82C), C15(H15A,
 H15B,H15C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C43(H43A,H43B,H43C),
 C49(H49A,H49B,H49C), C45(H45A,H45B,H45C), C12(H12A,H12B,H12C), C36(H36A,H36B,
 H36C), C3(H3A,H3B,H3C), C9(H9A,H9B,H9C), C41(H41A,H41B,H41C), C8(H8A,H8B,H8C),
 C44(H44A,H44B,H44C), C20(H20A,H20B,H20C), C37(H37A,H37B,H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'