Rhodium-Mediated Stereoselective Polymerization of "Carbenes"
Dennis G. H. Hetterscheid; Coen Hendriksen; Wojciech I. Dzik; Jan M. M. Smits; Ernst R. H. van Eck; Alan E. Rowan; Vincenzo Busico; Michele Vacatello; Valeria Van Axel Castelli; Annalaura Segre; Erica Jellema; Tom G. Bloemberg; Bas de Bruin; Journal of the American Chemical Society 128 (2006) 9746–9752; doi:10.1021/ja058722j

data_4110747
_publ_contact_author
;
        Dr. B. de Bruin
        Department of Homogeneous Catalysis
        Van 't Hoff Institute for Molecular Sciences
        University of Amsterdam
        Nieuwe Achtergracht 166
        1018 WV Amsterdam
        The Netherlands
;
_publ_contact_author_email       BdeBruin@science.uva.nl
_publ_contact_author_fax         '+31 20 525 6422'
_publ_contact_author_phone       '+31 20 525 6495'
_publ_section_title
;
 Rhodium-Mediated Stereoselective Polymerization of "Carbenes"
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9746
_journal_page_last               9752
_journal_paper_doi               10.1021/ja058722j
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C20 H26 Ir N O2'
_chemical_formula_weight         504.62
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-04-18
_audit_creation_method           'SHELXL, adapted and expanded'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0881(5)
_cell_length_b                   10.9092(4)
_cell_length_c                   17.6478(6)
_cell_measurement_reflns_used    330
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.190
_cell_volume                     1749.67(13)
_computing_data_collection
;
Nonius "Collect" program suite (Nonius, 1999)
;
_computing_data_reduction
;
Nonius "EvalCCD" program suite (Duisenberg, 1998)
;
_computing_molecular_graphics
;
PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF (Beurskens et al., 1996),
PATTY (Beurskens et al., 1987)
;
_diffrn_ambient_temperature      208(2)
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       'area detector \f and \w scan'
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19640
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0.000
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.643
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS multiscan (Sheldrick, 1996)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_description       'regular fragment'
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_Flack   0.047(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0137
_refine_ls_R_factor_gt           0.0124
_refine_ls_R_factor_obs          0.0124
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0080P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0256
_refine_ls_wR_factor_gt          0.0252
_refine_ls_wR_factor_obs         0.0252
_refine_ls_wR_factor_ref         0.0256
_reflns_number_gt                3891
_reflns_number_observed          3891
_reflns_number_total             3997
_reflns_observed_criterion       >2sigma(I)
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja058722jsi20060503_120158.cif
_cod_data_source_block           ERICA1
_cod_database_code               4110747