Homoleptic Trimethylsilylacetylide Complexes of Chromium(III), Iron(II), and Cobalt(III): Syntheses, Structures, and Ligand Field Parameters
Louise A. Berben; Jeffrey R. Long; Inorganic Chemistry 44 (2005) 8459–8468; doi:10.1021/ic051551z

data_4310021
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jrlong@berkeley.edu
_publ_contact_author_fax         '510 643-3832'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
Homoleptic Trimethylsilylacetylide Complexes of Chromium(III), Iron(II),
and Cobalt(III): Syntheses, Structures, and Ligand Field Parameters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8459
_journal_page_last               8468
_journal_paper_doi               10.1021/ic051551z
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        synthetic
_chemical_formula_structural
;
 [Li4Fe(CCSi(CH3)3)6](C4H10O)4(LiCCSi(CH3)3)4
;
_chemical_formula_sum            'C66 H130 Fe Li8 O4 Si10'
_chemical_formula_weight         1379.97
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.26(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.577(14)
_cell_length_b                   20.956(14)
_cell_length_c                   20.607(10)
_cell_measurement_reflns_used    90
_cell_measurement_temperature    293(2)
_cell_volume                     9069(10)
_computing_cell_refinement
;
  SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_reduction
;
  SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       'omega scans with profile analysis'
_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  0.1290
_diffrn_reflns_av_sigmaI/netI    0.1630
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32445
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.011
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'trapezoidal prism'
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(9)
_refine_ls_extinction_method
;
SHELXL 
 Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ 
;
_refine_ls_goodness_of_fit_all   0.986
_refine_ls_goodness_of_fit_obs   1.069
_refine_ls_hydrogen_treatment    construct
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         11035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_restrained_S_obs      1.069
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_obs          0.0650
_refine_ls_shift/esd_max         4.710
_refine_ls_shift/esd_mean        0.148
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1882
_refine_ls_wR_factor_obs         0.1407
_reflns_number_observed          5629
_reflns_number_total             11038
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic051551zsi20050910_072739.cif
_cod_data_source_block           lab50a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9069.9(94)
_cod_database_code               4310021