Indenyl- and Fluorenyl-Functionalized N-Heterocyclic Carbene Complexes of Titanium and Vanadium
Downing, Stephen P.; Danopoulos, Andreas A.; Organometallics 25 (2006) 1337–1340; doi:10.1021/om051017z

data_4074936
_publ_section_title
;
 Indenyl- and Fluorenyl-Functionalized N-Heterocyclic Carbene Complexes of
 Titanium and Vanadium
;
_journal_coden_ASTM              ORGND7
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1337
_journal_page_last               1340
_journal_paper_doi               10.1021/om051017z
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C30 H31 K N, C6 H6'
_chemical_formula_sum            'C36 H37 K N2'
_chemical_formula_weight         536.77
_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                 92.220(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.531(7)
_cell_length_b                   13.027(4)
_cell_length_c                   23.378(8)
_cell_measurement_reflns_used    2576
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.92
_cell_measurement_theta_min      2.26
_cell_volume                     6248(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
PLATON (Spek, 2003)
ENCIFER (Allen, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1992)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6868
_diffrn_reflns_av_R_equivalents  0.1136
_diffrn_reflns_av_sigmaI/netI    0.1046
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34299
_diffrn_reflns_theta_full        21.19
_diffrn_reflns_theta_max         21.19
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0133(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         7615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1773
_reflns_number_gt                4300
_reflns_number_total             7615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om051017zsi20060106_125724.cif
_cod_data_source_block           (Fl-NHC)-K+
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4074936