Wittig-Olefination via an Yttrium-Coordinated Betaine
Mark R. Crimmin; Andrew J. P. White; Chem.Commun. 48 (2012) 1745–; doi:10.1039/c2cc16431k

data_7107320
_publ_section_title
;
 Wittig-Olefination via an Yttrium-Coordinated Betaine
;
_journal_name_full               Chem.Commun.
_journal_page_first              1745
_journal_paper_doi               10.1039/c2cc16431k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C44 H63 I N2 O P Si4 Y'
_chemical_formula_sum            'C44 H63 I N2 O P Si4 Y'
_chemical_formula_weight         995.10
_chemical_name_common            'MRC I 065A1'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.687(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5750(4)
_cell_length_b                   24.9990(7)
_cell_length_c                   15.7491(4)
_cell_measurement_reflns_used    12477
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.0020
_cell_measurement_theta_min      2.9270
_cell_volume                     4948.8(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50239
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         32.07
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    1.964
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         15749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0329P)^2^+1.2197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                11490
_reflns_number_total             15749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc16431k.txt
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7107320