Transition-Metal-Catalyzed Bis-Silylation of Propyne by [2]Chromoarenophanes
Braunschweig, Holger; Kupfer, Thomas; Organometallics 26 (2007) 4634–; doi:10.1021/om700479h

data_4073579
_publ_section_title
;
 Transition-Metal-Catalyzed Bis-Silylation of Propyne by
 [2]Chromoarenophanes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4634
_journal_paper_doi               10.1021/om700479h
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C48 H68 Cr2 Li4 O6, C4 H8 O'
_chemical_formula_sum            'C52 H76 Cr2 Li4 O7'
_chemical_formula_weight         944.89
_chemical_name_common
;
?
;
_chemical_name_systematic
; 
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.776(2)
_cell_angle_beta                 90.841(2)
_cell_angle_gamma                93.436(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1815(4)
_cell_length_b                   12.3894(5)
_cell_length_c                   19.2910(7)
_cell_measurement_reflns_used    9307
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.10
_cell_volume                     2423.35(16)
_computing_cell_refinement       'Saint+ ver. 7.12A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 1.0-27 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.12A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            139675
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.64
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.9537
_exptl_absorpt_correction_T_min  0.8732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2004/1 (Brucker Nonius 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.589
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         13290
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+6.7877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.2116
_reflns_number_gt                9204
_reflns_number_total             13290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700479h-file002.cif
_cod_data_source_block           KR109
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073579