Osmium(II)-, Rhenium(I)-, and Tungsten(0)-Promoted Dipolar Cycloaddition Reactions with Pyrroles: Exploiting the Azomethine Ylide Character of This Heterocycle
Welch, Kevin D.; Smith, Philip L.; Keller, Andrew P.; Myers, William H.; Sabat, Michal; Harman, W. Dean; Organometallics 25 (2006) 5067–; doi:10.1021/om060586j

data_4074366
_publ_section_title
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 Osmium(II)-, Rhenium(I)-, and Tungsten(0)-Promoted Dipolar Cycloaddition
 Reactions with Pyrroles:&#x00A0; Exploiting the Azomethine Ylide
 Character of This Heterocycle
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_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5067
_journal_paper_doi               10.1021/om060586j
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C24 H36 B N8 O5 P W'
_chemical_formula_weight         742.24
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.7450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2690(10)
_cell_length_b                   16.1380(10)
_cell_length_c                   21.9880(10)
_cell_measurement_reflns_used    7246
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.010
_cell_measurement_theta_min      2.731
_cell_volume                     2919.5(4)
_computing_cell_refinement       'Bruker SMART'
_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 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker SMART APEX CCD detector'
_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     0.71074
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            20254
_diffrn_reflns_theta_full        32.52
_diffrn_reflns_theta_max         32.52
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    4.060
_exptl_absorpt_correction_T_max  0.821730
_exptl_absorpt_correction_T_min  0.660640
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.291
_refine_diff_density_min         -2.802
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         20254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                14122
_reflns_number_total             20254
_reflns_threshold_expression
'>2sigma(I) computing_data_collection Bruker SMART'
_cod_data_source_file            om060586jsi20060630_040706.cif
_cod_data_source_block           C24H36BN8O5PW
_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 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4074366