Stereoselective Synthesis oftrans-Tetrahydroindolines Promoted by a Tungsten π Base
MacLeod, Brianna L.; Pienkos, Jared A.; Myers, Jeffery T.; Sabat, Michal; Myers, William H.; Harman, W. Dean; Organometallics 33 (2014) 6286–; doi:10.1021/om501012q

data_4084669
_publ_section_title
;
 Stereoselective Synthesis oftrans-Tetrahydroindolines Promoted by a
 Tungsten \p Base
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6286
_journal_paper_doi               10.1021/om501012q
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C23 H33 B F3 N8 O4 P S W'
_chemical_formula_weight         800.26
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.2540(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2910(5)
_cell_length_b                   12.7130(4)
_cell_length_c                   16.0828(5)
_cell_measurement_reflns_used    9581
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      35.74
_cell_measurement_theta_min      3.61
_cell_volume                     3030.16(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0204
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41902
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.461
_exptl_absorpt_coefficient_mu    3.996
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.5545
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6174
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0169
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+2.0346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5710
_reflns_number_total             6174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501012q_si_002.cif
_cod_data_source_block           C23H33BF3N8O4PSW
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4084669--4084671.cif.
;
_cod_database_code               4084669
_shelx_estimated_absorpt_t_min   0.361
_shelx_estimated_absorpt_t_max   0.447
_shelxl_version_number           2013-3
_shelx_res_checksum              96343
_shelx_hkl_checksum              13605