#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:16:20 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178556 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/64/4066472.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4066472
loop_
_publ_author_name
'Chmely, Stephen C.'
'Hanusa, Timothy P.'
'Rheingold, Arnold L.'
_publ_section_title
;
 Influence of Ring Methylation in Group 15 Tetramethylcyclopentadienyl
 Complexes, M(C5Me4H)nI3−n(M = As, Sb)†
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5551
_journal_paper_doi               10.1021/om100474m
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C27 H39 Sb'
_chemical_formula_weight         485.33
_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                64.975(1)
_cell_angle_beta                 79.434(1)
_cell_angle_gamma                88.204(1)
_cell_formula_units_Z            2
_cell_length_a                   10.5877(15)
_cell_length_b                   10.8991(15)
_cell_length_c                   11.8207(16)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.48
_cell_volume                     1213.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22910
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0460P)²+2.2000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                3809
_reflns_number_total             4208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100474m_si_002.cif
_cod_data_source_block           vand52
_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_H-M      P-1
_cod_database_code               4066472
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sb1 Sb 0.947655(19) 0.77488(2) 0.16036(2) 0.02098(9) Uani 1 1 d .
C1 C 0.9396(3) 0.6476(3) 0.0532(3) 0.0223(7) Uani 1 1 d .
H1A H 1.0271 0.6245 0.0214 0.027 Uiso 1 1 calc R
C2 C 0.8760(3) 0.7394(3) -0.0524(3) 0.0222(7) Uani 1 1 d .
C3 C 0.7573(3) 0.6841(3) -0.0352(3) 0.0236(7) Uani 1 1 d .
C4 C 0.7412(3) 0.5512(3) 0.0744(3) 0.0236(7) Uani 1 1 d .
C5 C 0.8503(3) 0.5261(3) 0.1249(3) 0.0231(7) Uani 1 1 d .
C6 C 0.9377(4) 0.8706(4) -0.1573(3) 0.0273(8) Uani 1 1 d .
H6A H 0.8815 0.9094 -0.2198 0.041 Uiso 1 1 calc R
H6B H 1.0208 0.8532 -0.1988 0.041 Uiso 1 1 calc R
H6C H 0.9509 0.9345 -0.1215 0.041 Uiso 1 1 calc R
C7 C 0.6550(4) 0.7455(4) -0.1127(4) 0.0309(9) Uani 1 1 d .
H7A H 0.6867 0.8348 -0.1801 0.046 Uiso 1 1 calc R
H7B H 0.5778 0.7553 -0.0578 0.046 Uiso 1 1 calc R
H7C H 0.6339 0.6865 -0.1509 0.046 Uiso 1 1 calc R
C8 C 0.6215(3) 0.4602(4) 0.1197(3) 0.0284(8) Uani 1 1 d .
H8A H 0.6323 0.3771 0.1938 0.043 Uiso 1 1 calc R
H8B H 0.6061 0.4372 0.0515 0.043 Uiso 1 1 calc R
H8C H 0.5480 0.5071 0.1433 0.043 Uiso 1 1 calc R
C9 C 0.8815(4) 0.3986(4) 0.2297(4) 0.0277(8) Uani 1 1 d .
H9A H 0.8083 0.3324 0.2617 0.042 Uiso 1 1 calc R
H9B H 0.8990 0.4188 0.2988 0.042 Uiso 1 1 calc R
H9C H 0.9575 0.3612 0.1972 0.042 Uiso 1 1 calc R
C10 C 0.7352(3) 0.7591(3) 0.2263(3) 0.0222(7) Uani 1 1 d .
H10A H 0.6914 0.7243 0.1768 0.027 Uiso 1 1 calc R
C11 C 0.6984(3) 0.9012(3) 0.2013(3) 0.0247(8) Uani 1 1 d .
C12 C 0.6470(3) 0.9050(4) 0.3128(3) 0.0254(8) Uani 1 1 d .
C13 C 0.6382(3) 0.7674(3) 0.4151(3) 0.0239(7) Uani 1 1 d .
C14 C 0.6864(3) 0.6802(3) 0.3659(3) 0.0224(7) Uani 1 1 d .
C15 C 0.7151(4) 1.0135(4) 0.0690(4) 0.0328(9) Uani 1 1 d .
H15A H 0.6834 1.0972 0.0732 0.049 Uiso 1 1 calc R
H15B H 0.6663 0.9886 0.0182 0.049 Uiso 1 1 calc R
H15C H 0.8065 1.0277 0.0295 0.049 Uiso 1 1 calc R
C16 C 0.6010(4) 1.0269(4) 0.3338(4) 0.0348(9) Uani 1 1 d .
H16A H 0.5705 1.0001 0.4249 0.052 Uiso 1 1 calc R
H16B H 0.5304 1.0646 0.2880 0.052 Uiso 1 1 calc R
H16C H 0.6720 1.0955 0.3023 0.052 Uiso 1 1 calc R
C17 C 0.5845(4) 0.7337(4) 0.5520(4) 0.0333(9) Uani 1 1 d .
H17A H 0.5536 0.8159 0.5600 0.050 Uiso 1 1 calc R
H17B H 0.6518 0.6973 0.6025 0.050 Uiso 1 1 calc R
H17C H 0.5128 0.6659 0.5829 0.050 Uiso 1 1 calc R
C18 C 0.6884(3) 0.5289(4) 0.4324(4) 0.0302(8) Uani 1 1 d .
H18A H 0.6538 0.4988 0.5233 0.045 Uiso 1 1 calc R
H18B H 0.7771 0.5013 0.4210 0.045 Uiso 1 1 calc R
H18C H 0.6356 0.4876 0.3965 0.045 Uiso 1 1 calc R
C19 C 1.0352(3) 0.6389(4) 0.3253(3) 0.0242(8) Uani 1 1 d .
H19A H 0.9879 0.5492 0.3794 0.029 Uiso 1 1 calc R
C20 C 1.0479(3) 0.7261(4) 0.3927(3) 0.0261(8) Uani 1 1 d .
C21 C 1.1737(4) 0.7725(4) 0.3613(4) 0.0291(9) Uani 1 1 d .
C22 C 1.2476(3) 0.7168(4) 0.2798(4) 0.0320(9) Uani 1 1 d .
C23 C 1.1696(3) 0.6323(4) 0.2617(3) 0.0288(8) Uani 1 1 d .
C24 C 0.9388(4) 0.7555(4) 0.4761(4) 0.0341(9) Uani 1 1 d .
H24A H 0.9710 0.8117 0.5121 0.051 Uiso 1 1 calc R
H24B H 0.8997 0.6701 0.5451 0.051 Uiso 1 1 calc R
H24C H 0.8743 0.8039 0.4258 0.051 Uiso 1 1 calc R
C25 C 1.2321(4) 0.8635(4) 0.4071(4) 0.0440(11) Uani 1 1 d .
H25A H 1.1639 0.8937 0.4562 0.066 Uiso 1 1 calc R
H25B H 1.2769 0.9425 0.3338 0.066 Uiso 1 1 calc R
H25C H 1.2934 0.8134 0.4610 0.066 Uiso 1 1 calc R
C26 C 1.3898(4) 0.7475(5) 0.2273(4) 0.0430(11) Uani 1 1 d .
H26A H 1.4194 0.6965 0.1771 0.065 Uiso 1 1 calc R
H26B H 1.4366 0.7211 0.2977 0.065 Uiso 1 1 calc R
H26C H 1.4057 0.8448 0.1732 0.065 Uiso 1 1 calc R
C27 C 1.2098(4) 0.5457(4) 0.1927(4) 0.0372(9) Uani 1 1 d .
H27A H 1.3033 0.5564 0.1635 0.056 Uiso 1 1 calc R
H27B H 1.1671 0.5735 0.1194 0.056 Uiso 1 1 calc R
H27C H 1.1853 0.4505 0.2501 0.056 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C10 Sb1 C19 107.68(12)
C10 Sb1 C1 93.60(13)
C19 Sb1 C1 102.94(13)
C20 C19 C23 104.7(3)
C20 C19 Sb1 103.1(2)
C23 C19 Sb1 101.8(2)
C22 C23 C19 108.0(4)
C22 C23 C27 126.6(4)
C19 C23 C27 125.4(3)
C23 C22 C21 109.5(3)
C23 C22 C26 126.6(4)
C21 C22 C26 123.9(4)
C20 C21 C22 110.1(3)
C20 C21 C25 126.4(4)
C22 C21 C25 123.4(4)
C21 C20 C19 107.4(3)
C21 C20 C24 128.3(4)
C19 C20 C24 124.3(3)
C11 C10 C14 103.8(3)
C11 C10 Sb1 105.1(2)
C14 C10 Sb1 116.7(2)
C13 C14 C18 128.2(3)
C13 C14 C10 108.6(3)
C18 C14 C10 123.1(3)
C14 C13 C12 109.3(3)
C14 C13 C17 127.0(3)
C12 C13 C17 123.7(3)
C11 C12 C13 109.2(3)
C11 C12 C16 127.3(3)
C13 C12 C16 123.5(3)
C12 C11 C10 108.8(3)
C12 C11 C15 128.9(3)
C10 C11 C15 122.3(3)
C5 C1 C2 105.2(3)
C5 C1 Sb1 113.0(2)
C2 C1 Sb1 101.1(2)
C4 C5 C1 107.8(3)
C4 C5 C9 127.8(3)
C1 C5 C9 124.3(3)
C5 C4 C3 109.3(3)
C5 C4 C8 127.1(3)
C3 C4 C8 123.6(3)
C2 C3 C4 109.1(3)
C2 C3 C7 127.1(3)
C4 C3 C7 123.8(3)
C3 C2 C1 108.2(3)
C3 C2 C6 127.9(3)
C1 C2 C6 123.9(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sb1 C10 2.229(3)
Sb1 C19 2.234(3)
Sb1 C1 2.252(4)
C19 C20 1.497(5)
C19 C23 1.498(5)
C23 C22 1.362(5)
C23 C27 1.495(6)
C22 C21 1.448(6)
C22 C26 1.508(5)
C21 C20 1.367(5)
C21 C25 1.508(5)
C20 C24 1.495(6)
C10 C11 1.502(5)
C10 C14 1.497(5)
C14 C13 1.353(5)
C14 C18 1.499(5)
C13 C12 1.467(5)
C13 C17 1.499(5)
C12 C11 1.348(5)
C12 C16 1.504(5)
C11 C15 1.506(5)
C1 C5 1.484(5)
C1 C2 1.491(4)
C5 C4 1.364(5)
C5 C9 1.496(5)
C4 C3 1.467(5)
C4 C8 1.502(5)
C3 C2 1.354(5)
C3 C7 1.503(5)
C2 C6 1.507(5)
