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_4133169
_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         'I, 2(C6 H16 Cl Cr0.5 N2), C4 H8 O'
_chemical_formula_sum            'C16 H40 Cl2 Cr I N4 O'
_chemical_formula_weight         554.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.867(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.379(2)
_cell_length_b                   11.659(2)
_cell_length_c                   18.521(4)
_cell_measurement_reflns_used    2497
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.114
_cell_measurement_theta_min      2.256
_cell_volume                     2395.4(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, 2016)'
_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
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1572
_diffrn_reflns_av_unetI/netI     0.1732
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20541
_diffrn_reflns_theta_full        26.15
_diffrn_reflns_theta_max         26.15
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.001
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1147 before and 0.0545 after correction. The Ratio of minimum to maximum transmission is 0.7728. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.357
_refine_diff_density_min         -1.768
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4769
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1768
_refine_ls_R_factor_gt           0.1002
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+2.5386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                3009
_reflns_number_total             4769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b08739_si_009.cif
_cod_data_source_block           7
_cod_original_cell_volume        2395.5(8)
_cod_database_code               4133169
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'