Synthesis, Structure, and Reactivity of Rare-Earth Metallocene η3-Propargyl/Allenyl Complexes
Quiroga Norambuena, Victor F.; Heeres, André; Heeres, Hero J.; Meetsma, Auke; Teuben, Jan H.; Hessen, Bart; Organometallics 27 (2008) 5672–; doi:10.1021/om800547n

data_4072052
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Rare-Earth Metallocene
 \h3-Propargyl/Allenyl Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5672
_journal_paper_doi               10.1021/om800547n
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C29 H37 Y'
_chemical_formula_sum            'C29 H37 Y'
_chemical_formula_weight         474.52
_chemical_name_systematic        ' ?'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2003-06-03  08:08:02'
_audit_creation_method
;
 PLATON <TABLE ACC> option
 SHELXL97-2 & Manual Editing
;
_audit_update_record
;
 ?
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4646(9)
_cell_length_b                   10.5009(6)
_cell_length_c                   14.7315(8)
_cell_measurement_reflns_used    8011
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.30
_cell_volume                     2547.0(2)
_computing_cell_refinement       'SAINT, Bruker Version 6.02A, 2000'
_computing_data_collection       'SMART, Bruker Version 5.624, 2001'
_computing_data_reduction        'XPREP, Bruker Version 5.1/NT, 2000'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2003)
 PLATON (Spek, 1994)
;
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
  Bruker Smart Apex
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22023
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    2.302
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2000))'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
  Enantiomorph twin refinement resulted in 0.47(2) so ultimately set to 0.5
   Flack, H.D. & Bernardinelli, G. (1999, 2000)
;
_refine_ls_abs_structure_Flack   -0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6224
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                5315
_reflns_number_total             6224
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800547n_si_004.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4072052
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    8.3