Simple routes to bulky silyl-substituted acetylide ligands and examples of V(III), Fe(II), and Mn(II) complexes.
Yee, Gereon M.; Kowolik, Kristin; Manabe, Shuhei; Fettinger, James C.; Berben, Louise A.; Chemical communications (Cambridge, England) 47 (2011) 11680–11682; doi:10.1039/c1cc14758g

data_7112697
_publ_section_title
;
 Simple routes to bulky silyl-substituted acetylide ligands and examples
 of V(III), Fe(II), and Mn(II) complexes.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11680
_journal_page_last               11682
_journal_paper_doi               10.1039/c1cc14758g
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C64 H100 Fe Li2 O2 Si8, C5 H12'
_chemical_formula_sum            'C69 H112 Fe Li2 O2 Si8'
_chemical_formula_weight         1268.04
_chemical_name_systematic
;
?
;
_space_group_IT_number           1
_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
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_cell_angle_beta                 114.647(2)
_cell_angle_gamma                114.067(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3933(6)
_cell_length_b                   13.4814(6)
_cell_length_c                   14.5801(7)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      67.57
_cell_measurement_theta_min      4.25
_cell_volume                     1939.77(17)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2010-3) (Bruker, 2010)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_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      90(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX-II Duo CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
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_diffrn_reflns_av_R_equivalents  0.0000
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_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11875
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.9891
_exptl_absorpt_correction_T_min  0.9745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.07
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_refine_diff_density_max         0.598
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.146(12)
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         11884
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+0.3961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                11820
_reflns_number_total             11884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14758g.txt
_cod_data_source_block           gmy1tw51
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1939.78(16)
_cod_database_code               7112697