Reactions of Scorpionate-Anchored Yttrium and Lutetium Dialkyls with Terminal Alkynes: From Bimetallic Complexes with Bridging Enynediyl Ligands to Monomeric Terminal Dialkynyl Complexes†
Saliu, Kuburat O.; Cheng, Jianhua; McDonald, Robert; Ferguson, Michael J.; Takats, Josef; Organometallics 29 (2010) 4950–; doi:10.1021/om100393w

data_4066317
_publ_section_title
;
 Reactions of Scorpionate-Anchored Yttrium and Lutetium Dialkyls with
 Terminal Alkynes: From Bimetallic Complexes with Bridging Enynediyl
 Ligands to Monomeric Terminal Dialkynyl Complexes&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4950
_journal_paper_doi               10.1021/om100393w
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C109 H156 B Lu N6 O, 3.5(C5 H12)'
_chemical_formula_sum            'C126.5 H198 B Lu N6 O'
_chemical_formula_weight         2004.69
_chemical_name_systematic
; 
 ? 
;
_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                 100.034(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2069(14)
_cell_length_b                   37.457(4)
_cell_length_c                   23.450(2)
_cell_measurement_reflns_used    8086
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.08
_cell_volume                     12288(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w 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  0.1127
_diffrn_reflns_av_sigmaI/netI    0.1101
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81486
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  0.9507
_exptl_absorpt_correction_T_min  0.7905
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4332
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered
 or partial-occupancy solvent pentane carbon atoms were
 unsuccessful.  The data were corrected for disordered electron density
 through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L.
 Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek,
 A.L. Acta Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst.
 2003, 36, 7-13.  PLATON - a multipurpose crystallographic tool.
 Utrecht University, Utrecht, The Netherlands).  A total
 solvent-accessible void volume of 2825 A3 with a total electron count
 of 611 (consistent with 14 molecules of solvent pentane, or 3.5 molecules
 per formula unit of the Lu complex) was found in the unit cell.
;
_refine_diff_density_max         1.071
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1147
_refine_ls_number_reflns         22230
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                13586
_reflns_number_total             22230
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om100393w_si_002.cif
_cod_data_source_block           11-Lu
_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 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C126.50 H198 B Lu N6 O'
_cod_database_code               4066317