Amine Elimination Reactions between Homoleptic Silylamide Lanthanide Complexes and an Isopropylidene-Bridged Cyclopentadiene−Fluorene System
Dash, Aswini K.; Razavi, Abbas; Mortreux, André; Lehmann, Christian W.; Carpentier, Jean-François; Organometallics 21 (2002) 3238–; doi:10.1021/om0200398

data_4076799
_publ_section_title
;
 Amine Elimination Reactions between Homoleptic Silylamide Lanthanide
 Complexes and an Isopropylidene-Bridged Cyclopentadiene&#x2212;Fluorene
 System
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3238
_journal_paper_doi               10.1021/om0200398
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source        'see paper'
_chemical_formula_sum            'C52 H57 La O2.5'
_chemical_formula_weight         860.89
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     Patterson
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.7740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0242(7)
_cell_length_b                   16.7576(6)
_cell_length_c                   13.3536(5)
_cell_measurement_reflns_used    6587
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.17
_cell_measurement_theta_min      1.88
_cell_volume                     4256.7(3)
_computing_cell_refinement       'SMART software (Siemens, 1995)'
_computing_data_collection       'SMART software (Siemens, 1995)'
_computing_data_reduction        'SAINT software (Siemens, 1995)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'CCD \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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0765
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46450
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         33.17
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'XPREP, Siemens (1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.74
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.531
_refine_diff_density_min         -2.404
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         15356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0769
_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^)+(0.0894P)^2^+20.2609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                10388
_reflns_number_total             15356
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om0200398.cif
_cod_data_source_block           3687_La_complex_12.THF(THF)1.5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_formula_sum        'C52 H57 La O2.50'
_cod_database_code               4076799