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_4070316
_publ_section_title
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 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            'C19 H29 B F3 N8 O4 P S W'
_chemical_formula_weight         748.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.9570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8772(3)
_cell_length_b                   8.4775(2)
_cell_length_c                   27.0201(6)
_cell_measurement_reflns_used    5250
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.26
_cell_volume                     2720.25(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0499
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_exptl_absorpt_coefficient_mu    4.445
_exptl_absorpt_correction_T_max  0.7175
_exptl_absorpt_correction_T_min  0.3217
_exptl_absorpt_correction_type   'multiple scans'
_exptl_absorpt_process_details   'Bruker Scale'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.268
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                4315
_reflns_number_total             5307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900714r_si_002.cif
_cod_data_source_block           C19H29BF3N8O4PSW
_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 

The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'monoclinc' was replaced with
'monoclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4070316