Synthesis ofN-(2-Pyranyl)- andN-Cyclohexylindole Derivatives via Stereoselective Addition of Indole Nucleophiles to Organomolybdenum Complexes
Bjurling, Emelie; Johansson, Maria H.; Andersson, Carl-Magnus; Organometallics 18 (1999) 5606–; doi:10.1021/om9906060

data_4077828
_publ_section_title
;
 Synthesis ofN-(2-Pyranyl)- andN-Cyclohexylindole Derivatives via
 Stereoselective Addition of Indole Nucleophiles to Organomolybdenum
 Complexes
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5606
_journal_paper_doi               10.1021/om9906060
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C21 H16 Mo N2 O3'
_chemical_formula_weight         440.30
_chemical_name_systematic
; 
 (\n^5^-Cyclopentadienyl)(dicarbonyl)-[(3,4,5-\n)-2-anti-(3-cyanoindol-1-yl)-
5,6-dihydro-2H-pyran-5-yl]molybdenum 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   'riding model'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.575(4)
_cell_length_b                   14.910(3)
_cell_length_c                   12.837(3)
_cell_measurement_reflns_used    7712
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     3643.0(17)
_computing_cell_refinement       'Bruker SMART CCD system'
_computing_data_collection       'Bruker SMART CCD system'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1997)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'SMART CCD system'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17867
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         32.19
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_correction_T_min  0.8715
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'absorption corrections using SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                4284
_reflns_number_total             5824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9906060.cif
_cod_data_source_block           OM_9906060
_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        3642.9(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4077828