Michael−Aldol Ring Closures with Dihapto-Coordinated Pyrrole Complexes and the Synthesis of Tetrahydroindole Cores
Welch, Kevin D.; Harrison, Daniel P.; Sabat, Michal; Hejazi, Emily Z.; Parr, Brendan T.; Fanelli, Matthew G.; Gianfrancesco, Nicole A.; Nagra, Dalsher S.; Myers, William H.; Harman, W. Dean; Organometallics 28 (2009) 5960–; doi:10.1021/om900714r

data_4070315
_publ_section_title
;
 Michael&#x2212;Aldol Ring Closures with Dihapto-Coordinated Pyrrole
 Complexes and the Synthesis of Tetrahydroindole Cores
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5960
_journal_paper_doi               10.1021/om900714r
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C24 H36 B N8 O3 P W'
_chemical_formula_weight         710.24
_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                 90.92(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.060(2)
_cell_length_b                   11.610(2)
_cell_length_c                   22.088(4)
_cell_measurement_reflns_used    7905
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      17.421
_cell_measurement_theta_min      2.698
_cell_volume                     2835.9(9)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            25995
_diffrn_reflns_theta_full        36.43
_diffrn_reflns_theta_max         36.43
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    4.171
_exptl_absorpt_correction_T_max  0.89743
_exptl_absorpt_correction_T_min  0.56871
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.713
_refine_diff_density_min         -1.539
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         13485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                11434
_reflns_number_total             13485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900714r_si_001.cif
_cod_data_source_block           C22H33BN8O2PW-acetone
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2835.9(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070315