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_4084671
_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            'C27 H40 B N8 O2 P W'
_chemical_formula_weight         734.30
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 106.782(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.105(2)
_cell_length_b                   11.767(2)
_cell_length_c                   19.260(3)
_cell_measurement_reflns_used    9467
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      36.70
_cell_measurement_theta_min      3.48
_cell_volume                     3060.5(8)
_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      233(2)
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0145
_diffrn_reflns_av_unetI/netI     0.0083
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41489
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.376
_exptl_absorpt_coefficient_mu    3.865
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.5689
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6244
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0143
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+2.5126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0348
_refine_ls_wR_factor_ref         0.0362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5982
_reflns_number_total             6244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501012q_si_002.cif
_cod_data_source_block           C27H40BN8O2PW
_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_original_cell_volume        3060.6(9)
_cod_database_code               4084671
_shelx_estimated_absorpt_t_min   0.287
_shelx_estimated_absorpt_t_max   0.411
_shelxl_version_number           2013-4
_shelx_res_checksum              22110
_shelx_hkl_checksum              37891