Towards taxane analogues synthesis by dienyne ring closing metathesis
Pérez-Estrada, S.; Sayar, N.; Granja, J. R.; Organic Chemistry Frontiers 3 (2016) 1331–; doi:10.1039/C6QO00321D

data_1553493
_publ_section_title
;
 Towards taxane analogues synthesis by dienyne ring closing metathesis
;
_journal_issue                   10
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1331
_journal_paper_doi               10.1039/C6QO00321D
_journal_volume                  3
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H40 O5 Si'
_chemical_formula_sum            'C29 H40 O5 Si'
_chemical_formula_weight         496.7
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2016-06-10T13:34:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-07-01 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.711(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.836(4)
_cell_length_b                   7.8125(10)
_cell_length_c                   14.1759(19)
_cell_measurement_reflns_used    5155
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.71
_cell_measurement_wavelength     0.71073
_cell_volume                     3079.4(7)
_computing_cell_refinement       'SAINT V8.37A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'SMART 1000 CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'fixed \k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w oscillation scans'
_diffrn_orient_matrix_UB_11      -0.012017
_diffrn_orient_matrix_UB_12      -0.1191
_diffrn_orient_matrix_UB_13      0.009484
_diffrn_orient_matrix_UB_21      -0.007093
_diffrn_orient_matrix_UB_22      0.02879
_diffrn_orient_matrix_UB_23      0.066653
_diffrn_orient_matrix_UB_31      -0.033147
_diffrn_orient_matrix_UB_32      0.037018
_diffrn_orient_matrix_UB_33      -0.021324
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19413
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.99
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.943
_diffrn_reflns_theta_min         1.465
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol, Hexane'
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 2416 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     404
_refine_ls_number_reflns         7333
_refine_ls_number_restraints     395
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0439P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                6089
_reflns_number_total             7333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qo00321d2.cif
_cod_data_source_block           Compound21
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               1553493
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              46355
_shelx_hkl_checksum              87553
_shelx_fab_checksum              69373