Synthesis of a stibindolyl anion from trimesitylantimony and potassium
Breunig, Hans Joachim; Ghesner, Mihaiela Emilia; Lork, Enno; Chemical Communications (Cambridge, United Kingdom)  (2003) 274–275; doi:10.1039/b211177b

data_7113527
_publ_section_title
;
 Synthesis of a stibindolyl anion from trimesitylantimony and potassium
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   2
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              274
_journal_page_last               275
_journal_paper_doi               10.1039/b211177b
_journal_year                    2003
_chemical_formula_sum            'C27 H41 K N3 Sb'
_chemical_formula_weight         568.48
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 105.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.681(5)
_cell_length_b                   9.641(2)
_cell_length_c                   13.243(3)
_cell_measurement_reflns_used    800
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.03
_cell_volume                     2909.4(12)
_computing_cell_refinement       'STOE Cell'
_computing_data_collection       'STOE Expose'
_computing_data_reduction        'STOE Integrate'
_computing_molecular_graphics    'Siemens SHELXTL / DIAMOND'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS'
_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  0.1266
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35681
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        'random variation +/-2.0'
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Stuart & Walker, Acta Cryst A (1983)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                3324
_reflns_number_total             5123
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103940
_cod_data_source_file            b211177b.txt
_cod_data_source_block           COMPOUND_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'refdelF' changed to 'refdelf'
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        2909.4(11)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7113527