Diazomethane Insertion into Lanthanide− and Yttrium−C(allyl) Bonds To Form the η2-Hydrazonato Complexes (C5Me5)2Ln[η2(N,N′)-RNNCHSiMe3] (R = C3H5)
Evans, William J.; Montalvo, Elizabeth; Champagne, Timothy M.; Ziller, Joseph W.; DiPasquale, Antonio G.; Rheingold, Arnold L.; Organometallics 27 (2008) 3582–; doi:10.1021/om800065j

data_4071262
_publ_section_title
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 Diazomethane Insertion into Lanthanide&#x2212; and
 Yttrium&#x2212;C(allyl) Bonds To Form the \h2-Hydrazonato Complexes
 (C5Me5)2Ln[\h2(N,N&#x2032;)-RNNCHSiMe3] (R = C3H5)
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3582
_journal_paper_doi               10.1021/om800065j
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C27 H45 La N2 Si'
_chemical_formula_weight         564.65
_chemical_name_common            emA
_chemical_name_systematic
;
 ?
;
_space_group.centring_type       P
_space_group_IT_number           14
_space_group.IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.539(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5050(18)
_cell_length_b                   14.053(2)
_cell_length_c                   17.978(3)
_cell_measurement_reflns_used    6392
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.32
_cell_volume                     2837.4(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_refln_scan_rate          10
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23844
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_T_max  0.9401
_exptl_absorpt_correction_T_min  0.8594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         6573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0211P)^2^+3.3356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                5707
_reflns_number_total             6573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800065j-file001.cif
_cod_data_source_block           complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_space_group.centring_type' value 'primitive' was replaced with the
value 'P' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_original_cell_volume        2837.3(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4071262