Synthesis and Complexation Behavior of Indenyl and Cyclopentadienyl Ligands Functionalized with a Naphthyridine Unit
Sieb, David; Schuhen, Katrin; Morgen, Michael; Herrmann, Heike; Wadepohl, Hubert; Lucas, Nigel T.; Baker, Robert W.; Enders, Markus; Organometallics 31 (2012) 356–; doi:10.1021/om2009638

data_4067961
_publ_section_title
;
 Synthesis and Complexation Behavior of Indenyl and Cyclopentadienyl
 Ligands Functionalized with a Naphthyridine Unit
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              356
_journal_paper_doi               10.1021/om2009638
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C25 H29 N2 Rh'
_chemical_formula_weight         460.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                en_ds14
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.286(12)
_cell_angle_beta                 93.244(16)
_cell_angle_gamma                100.350(12)
_cell_formula_units_Z            4
_cell_length_a                   8.832(4)
_cell_length_b                   14.909(6)
_cell_length_c                   17.469(8)
_cell_measurement_reflns_used    7488
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.36
_cell_measurement_theta_min      2.36
_cell_volume                     2057.7(16)
_computing_cell_refinement
;
SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2008)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD-PXL-KAF2 (Bruker AXS Smart 1000)'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            50193
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.36
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.971
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         12526
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+5.3639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                8307
_reflns_number_total             12526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2009638_si_001.cif
_cod_data_source_block           8
_cod_original_cell_volume        2057.5(16)
_cod_database_code               4067961
_audit_block_refno               934