Synthesis and reaction of [(Tp(iPr2))LnH2]3 (Ln = Y, Lu) with CO: trinuclear cluster-bound propenolate en route to selective formation of propene.
Cheng, Jianhua; Ferguson, Michael J.; Takats, Josef; Journal of the American Chemical Society 132 (2010) 2–3; doi:10.1021/ja905679k

data_4101622
_publ_section_title
;
 Synthesis and reaction of [(Tp(iPr2))LnH2]3 (Ln = Y, Lu) with CO:
 trinuclear cluster-bound propenolate en route to selective formation of
 propene.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2
_journal_page_last               3
_journal_paper_doi               10.1021/ja905679k
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C87 H158 B3 N18 Y3'
_chemical_formula_weight         1755.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8240(11)
_cell_length_b                   18.0259(11)
_cell_length_c                   31.3594(19)
_cell_measurement_reflns_used    9313
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.26
_cell_volume                     10075.6(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            89564
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.762
_exptl_absorpt_correction_T_max  0.5125
_exptl_absorpt_correction_T_min  0.4323
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3752
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.44
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered or
partial-occupancy solvent hexane 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, 194201) as implemented in PLATON (Spek, A.L. Acta
Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 713.
PLATON - a multipurpose crystallographic tool.  Utrecht University,
Utrecht, The Netherlands).  A total solvent-accessible void volume of
1163 A3 with a total electron count of 240 (consistent with 4 molecules
of solvent hexane, or 1 molecule per formula unit of the
[{HB(3,5-iPr2-pyrazolyl)3}3Y3(H)6] molecule) was found in the unit cell.
;
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881. 10893 Friedel pairs'
_refine_ls_abs_structure_Flack   0.003(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         23954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                20422
_reflns_number_total             23954
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja905679k_si_001.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 
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_cod_database_code               4101622