# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'G Reid'
'Marek Jura'
'W Levason'
'Michael Webster'

_publ_contact_author_name        'G Reid'
_publ_contact_author_email       GR@SOTON.AC.UK

_publ_section_title              
;
Preparation and properties of cyclic and open-chain
Sb/N-donor ligands
;

# Attachment 'SbN_all4_1.cif'

# Manuscript ref.:
# Title: Preparation and properties of cyclic and open-chain Sb/N-donor ligands
# Authors: M. Jura, W. Levason, G. Reid and M. Webster
# Journal (proposed): Dalton Trans.
# CCDC ref. no(s).:
# DOI:
#
##############################################################################
### CIF submission form for molecular structure report ###
### Version: 2.0.2 (6 July 1998). (Updated 20-Apr-2005) ###
##############################################################################

# This is an electronic "form" for submitting structural details as a
# Crystallographic Information File (CIF).
# Full details of the format of such files are given in the paper "The
# Crystallographic Information File (CIF): a New Standard Archive File for
# Crystallography" by S. R. Hall, F. H. Allen and I. D. Brown [Acta Cryst.
# (1991), A47, 655-685].
#
# CIFs can be checked for legal syntax and possible errors (ALERTS) by
# using checkcif software at:
# http://journals.iucr.org/services/cif/checkcif.html
# http://journals.iucr.org/services/cif/checking/checkstructural.html
# http://checkcif.iucr.org (produces o/p in pdf or html format).
#
#==============================================================================
data_08mj55
_database_code_depnum_ccdc_archive 'CCDC 731685'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2008-12-03
_audit_author_name               'Webster, M.'

_chemical_name_systematic        
;
{propane-1,3-diylbis[(methylimino)methylene-2,1-phenylene]}-
bis(trimethylstibonium) iodide chloroform solvate
;

# 'C25 H42 N2 Sb2 2+ cation name from iLab software.

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H42 N2 Sb2 2+, 0.333(C H Cl3), 2(I 1-)'
_chemical_formula_sum            'C25.333 H42.333 Cl I2 N2 Sb2'
_chemical_formula_weight         907.70

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'
N N 0.0061 0.0033 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'

_cell_length_a                   13.7732(10)
_cell_length_b                   13.7732(10)
_cell_length_c                   29.544(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4853.6(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3604
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2600
_exptl_absorpt_coefficient_mu    3.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6283 # 0.7829
_exptl_absorpt_correction_T_max  1.0000 # 0.9301
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28258
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3789
_reflns_number_gt                3106
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0071P)^2^+10.3781P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3789
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0636
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.3333 0.6667 0.42716(2) 0.03077(14) Uani 1 3 d S . .
I2 I 0.70642(4) -0.00713(5) 0.2500 0.02872(12) Uani 1 2 d S . .
I3 I 0.0000 0.0000 0.41596(5) 0.0608(4) Uani 0.50 3 d SP A 1
Sb1 Sb 0.09945(3) 0.32996(4) 0.357659(11) 0.03147(10) Uani 1 1 d . . .
N1 N -0.0857(4) 0.3613(4) 0.33507(15) 0.0234(10) Uani 1 1 d . . .
C1 C 0.1849(5) 0.4777(5) 0.3187(2) 0.0339(14) Uani 1 1 d . . .
H1A H 0.2168 0.5431 0.3388 0.051 Uiso 1 1 calc R . .
H1B H 0.1323 0.4822 0.2976 0.051 Uiso 1 1 calc R . .
H1C H 0.2453 0.4765 0.3016 0.051 Uiso 1 1 calc R . .
C2 C 0.2347(5) 0.3163(7) 0.3837(2) 0.0464(19) Uani 1 1 d . . .
H2A H 0.2750 0.3053 0.3587 0.070 Uiso 1 1 calc R . .
H2B H 0.2061 0.2522 0.4044 0.070 Uiso 1 1 calc R . .
H2C H 0.2858 0.3851 0.4001 0.070 Uiso 1 1 calc R . .
C3 C 0.0041(5) 0.1824(4) 0.3202(2) 0.0332(13) Uani 1 1 d . . .
H3A H 0.0543 0.1660 0.3024 0.050 Uiso 1 1 calc R . .
H3B H -0.0463 0.1923 0.2997 0.050 Uiso 1 1 calc R . .
H3C H -0.0401 0.1200 0.3409 0.050 Uiso 1 1 calc R . .
C4 C 0.0176(5) 0.3381(5) 0.41705(16) 0.0323(12) Uani 1 1 d . . .
C5 C 0.0774(5) 0.3626(6) 0.45764(19) 0.0451(18) Uani 1 1 d . . .
H5 H 0.1514 0.3740 0.4579 0.054 Uiso 1 1 calc R . .
C6 C 0.0287(5) 0.3703(5) 0.49779(18) 0.0397(15) Uani 1 1 d . . .
H6 H 0.0694 0.3880 0.5254 0.048 Uiso 1 1 calc R . .
C7 C -0.0788(5) 0.3522(5) 0.4971(2) 0.0358(15) Uani 1 1 d . . .
H7 H -0.1124 0.3569 0.5245 0.043 Uiso 1 1 calc R . .
C8 C -0.1396(5) 0.3270(5) 0.45670(18) 0.0304(12) Uani 1 1 d . . .
H8 H -0.2138 0.3150 0.4567 0.036 Uiso 1 1 calc R . .
C9 C -0.0911(5) 0.3194(5) 0.41644(17) 0.0274(12) Uani 1 1 d . . .
C10 C -0.1563(4) 0.2906(5) 0.37274(18) 0.0278(12) Uani 1 1 d . . .
H10A H -0.1847 0.2107 0.3654 0.033 Uiso 1 1 calc R . .
H10B H -0.2216 0.3016 0.3764 0.033 Uiso 1 1 calc R . .
C11 C -0.1492(4) 0.3232(5) 0.29226(17) 0.0260(12) Uani 1 1 d . . .
H11A H -0.2075 0.3452 0.2922 0.031 Uiso 1 1 calc R . .
H11B H -0.1878 0.2403 0.2911 0.031 Uiso 1 1 calc R . .
C12 C -0.0515(5) 0.4792(5) 0.34372(19) 0.0325(12) Uani 1 1 d . . .
H12A H -0.0070 0.5253 0.3181 0.049 Uiso 1 1 calc R . .
H12B H -0.0063 0.5045 0.3714 0.049 Uiso 1 1 calc R . .
H12C H -0.1183 0.4865 0.3474 0.049 Uiso 1 1 calc R . .
C13 C -0.0780(6) 0.3698(7) 0.2500 0.0278(18) Uani 1 2 d S . .
H13A H -0.0419 0.4526 0.2500 0.033 Uiso 1 2 calc SR . .
H13B H -0.0182 0.3499 0.2500 0.033 Uiso 1 2 calc SR . .
Cl1 Cl -0.0936(3) -0.1370(3) 0.44793(17) 0.0707(13) Uani 0.50 1 d P B 2
C14 C 0.0000 0.0000 0.4644(6) 0.031(4) Uani 0.50 3 d SP . 2
H14 H 0.0000 0.0000 0.5000 0.037 Uiso 1 6 d S C 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.03199(19) 0.03199(19) 0.0283(3) 0.000 0.000 0.01600(10)
I2 0.0302(3) 0.0268(2) 0.0309(2) 0.000 0.000 0.0155(2)
I3 0.0739(7) 0.0739(7) 0.0346(8) 0.000 0.000 0.0370(4)
Sb1 0.01980(18) 0.0460(2) 0.02146(16) 0.0004(2) 0.00175(16) 0.01109(18)
N1 0.023(2) 0.023(2) 0.024(2) -0.0037(19) -0.001(2) 0.0108(19)
C1 0.026(3) 0.029(3) 0.031(3) -0.001(3) 0.013(3) 0.001(2)
C2 0.026(3) 0.075(6) 0.035(3) 0.007(4) 0.002(3) 0.022(4)
C3 0.021(3) 0.027(3) 0.049(4) 0.003(3) 0.003(3) 0.010(3)
C4 0.032(3) 0.042(3) 0.022(2) 0.005(3) 0.005(2) 0.018(3)
C5 0.024(3) 0.068(5) 0.028(3) 0.005(3) 0.003(3) 0.012(3)
C6 0.034(4) 0.054(4) 0.021(3) 0.007(3) 0.000(3) 0.014(3)
C7 0.042(4) 0.030(3) 0.030(3) 0.009(3) 0.012(3) 0.014(3)
C8 0.026(3) 0.029(3) 0.033(3) 0.005(3) 0.011(3) 0.011(3)
C9 0.025(3) 0.025(3) 0.024(3) 0.005(2) 0.006(2) 0.007(3)
C10 0.019(3) 0.032(3) 0.032(3) 0.002(3) 0.003(2) 0.013(2)
C11 0.022(3) 0.032(3) 0.025(3) -0.001(3) -0.001(2) 0.014(3)
C12 0.040(3) 0.028(3) 0.033(3) -0.003(3) 0.005(3) 0.019(3)
C13 0.023(4) 0.031(4) 0.031(4) 0.000 0.000 0.016(3)
Cl1 0.053(2) 0.0417(19) 0.111(4) -0.010(2) -0.029(2) 0.0192(17)
C14 0.034(6) 0.034(6) 0.025(10) 0.000 0.000 0.017(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 C3 2.101(6) . ?
Sb1 C2 2.109(6) . ?
Sb1 C1 2.112(6) . ?
Sb1 C4 2.119(5) . ?
N1 C12 1.470(7) . ?
N1 C11 1.477(6) . ?
N1 C10 1.478(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C9 1.387(7) . ?
C4 C5 1.397(7) . ?
C5 C6 1.393(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.372(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.399(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.508(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C13 1.518(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C11 1.518(7) 10_556 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
Cl1 C14 1.740(6) . ?
C14 Cl1 1.740(6) 3 ?
C14 Cl1 1.740(6) 5 ?
C14 H14 1.051(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Sb1 C2 105.0(3) . . ?
C3 Sb1 C1 115.0(2) . . ?
C2 Sb1 C1 101.1(3) . . ?
C3 Sb1 C4 113.3(2) . . ?
C2 Sb1 C4 102.7(2) . . ?
C1 Sb1 C4 117.1(2) . . ?
C12 N1 C11 110.3(4) . . ?
C12 N1 C10 109.8(4) . . ?
C11 N1 C10 109.5(4) . . ?
Sb1 C1 H1A 109.5 . . ?
Sb1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Sb1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Sb1 C2 H2A 109.5 . . ?
Sb1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Sb1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Sb1 C3 H3A 109.5 . . ?
Sb1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Sb1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C9 C4 C5 120.5(5) . . ?
C9 C4 Sb1 122.2(4) . . ?
C5 C4 Sb1 117.3(4) . . ?
C6 C5 C4 120.0(6) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C7 C6 C5 119.4(6) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 121.0(6) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C7 119.8(5) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C4 C9 C8 119.2(5) . . ?
C4 C9 C10 120.3(5) . . ?
C8 C9 C10 120.4(5) . . ?
N1 C10 C9 111.2(4) . . ?
N1 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
N1 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N1 C11 C13 114.3(4) . . ?
N1 C11 H11A 108.7 . . ?
C13 C11 H11A 108.7 . . ?
N1 C11 H11B 108.7 . . ?
C13 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 C11 110.7(6) 10_556 . ?
C11 C13 H13A 109.5 10_556 . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 10_556 . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
Cl1 C14 Cl1 112.5(5) . 3 ?
Cl1 C14 Cl1 112.5(5) . 5 ?
Cl1 C14 Cl1 112.5(5) 3 5 ?
Cl1 C14 H14 106.3(6) . . ?
Cl1 C14 H14 106.3(6) 3 . ?
Cl1 C14 H14 106.3(6) 5 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.138

#===END OF CIF ==============================================================
# 08mj40

data_08mj40
_database_code_depnum_ccdc_archive 'CCDC 731686'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2009-01-07
_audit_author_name               'Webster, M.'

_chemical_name_systematic        
;
bis(bis(N-(2-(dimethylstibanyl)benzyl))-methanamine-Sb,Sb')-
copper(I) tetrafluoroborate
;

# iLab IUPAC name of ligand:
# N-[2-(dimethylstibino)benzyl]-1-[2-(dimethylstibino)phenyl]-
# N-methylmethanamine
#
# How about bis(N-(2-(dimethylstibanyl)benzyl))-methanamine for ligand.
# bis(bis(N-(2-(dimethylstibanyl)benzyl))-methanamine-Sb,Sb')-
# copper(I) tetrafluoroborate
#
# bis(N-[2-(dimethylstibino)benzyl]-1-[2-(dimethylstibino)phenyl]-
# N-methylmethanamine-Sb,Sb')copper(I) tetrafluoroborate

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H54 Cu N2 Sb4 1+, B F4 1-'
_chemical_formula_sum            'C38 H54 B Cu F4 N2 Sb4'
_chemical_formula_structural     '((C19 H27 N Sb2)2 Cu) (B F4)'
_chemical_formula_weight         1176.18

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.517(3)
_cell_length_b                   20.044(4)
_cell_length_c                   14.2102(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.588(10)
_cell_angle_gamma                90.00
_cell_volume                     4313.5(13) # shelxl .7(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    50216
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2280
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6281 # 0.5850
_exptl_absorpt_correction_T_max  0.7456 # 0.8893
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            53978
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9867
_reflns_number_gt                6854
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+14.1381P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9867
_refine_ls_number_parameters     461
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.24654(5) 0.39887(4) 0.72361(5) 0.02030(17) Uani 1 1 d . . .
Sb1 Sb 0.28232(3) 0.48338(2) 0.60559(3) 0.02117(10) Uani 1 1 d . . .
Sb2 Sb 0.36958(3) 0.31420(2) 0.73613(3) 0.02248(10) Uani 1 1 d . . .
Sb3 Sb 0.10134(3) 0.34122(2) 0.65573(3) 0.02705(11) Uani 1 1 d . . .
Sb4 Sb 0.23351(3) 0.44502(2) 0.88625(3) 0.02312(11) Uani 1 1 d . . .
N1 N 0.4655(3) 0.5042(2) 0.7315(3) 0.0210(11) Uani 1 1 d . . .
N2 N 0.0589(3) 0.5086(3) 0.8014(3) 0.0236(11) Uani 1 1 d . . .
C1 C 0.3696(5) 0.4686(3) 0.5113(4) 0.0330(16) Uani 1 1 d . . .
H1A H 0.3908 0.5120 0.4938 0.049 Uiso 1 1 calc R . .
H1B H 0.3383 0.4457 0.4529 0.049 Uiso 1 1 calc R . .
H1C H 0.4199 0.4415 0.5437 0.049 Uiso 1 1 calc R . .
C2 C 0.1694(5) 0.5010(3) 0.4921(5) 0.0389(18) Uani 1 1 d . . .
H2A H 0.1831 0.5359 0.4494 0.058 Uiso 1 1 calc R . .
H2B H 0.1198 0.5153 0.5197 0.058 Uiso 1 1 calc R . .
H2C H 0.1536 0.4598 0.4553 0.058 Uiso 1 1 calc R . .
C3 C 0.3065(4) 0.5854(3) 0.6515(4) 0.0209(13) Uani 1 1 d . . .
C4 C 0.2576(4) 0.6366(3) 0.5994(4) 0.0279(15) Uani 1 1 d . . .
H4 H 0.2139 0.6266 0.5432 0.033 Uiso 1 1 calc R . .
C5 C 0.2723(4) 0.7029(3) 0.6292(5) 0.0302(15) Uani 1 1 d . . .
H5 H 0.2387 0.7376 0.5932 0.036 Uiso 1 1 calc R . .
C6 C 0.3352(4) 0.7179(3) 0.7105(5) 0.0330(17) Uani 1 1 d . . .
H6 H 0.3455 0.7630 0.7302 0.040 Uiso 1 1 calc R . .
C7 C 0.3833(4) 0.6675(3) 0.7635(4) 0.0257(14) Uani 1 1 d . . .
H7 H 0.4265 0.6783 0.8197 0.031 Uiso 1 1 calc R . .
C8 C 0.3695(4) 0.6007(3) 0.7357(4) 0.0222(13) Uani 1 1 d . . .
C9 C 0.4238(4) 0.5469(3) 0.7932(4) 0.0228(13) Uani 1 1 d . . .
H9A H 0.4701 0.5673 0.8440 0.027 Uiso 1 1 calc R . .
H9B H 0.3856 0.5192 0.8251 0.027 Uiso 1 1 calc R . .
C10 C 0.5264(4) 0.5451(3) 0.6893(5) 0.0313(16) Uani 1 1 d . . .
H10A H 0.5747 0.5611 0.7407 0.047 Uiso 1 1 calc R . .
H10B H 0.4944 0.5833 0.6554 0.047 Uiso 1 1 calc R . .
H10C H 0.5506 0.5180 0.6437 0.047 Uiso 1 1 calc R . .
C11 C 0.5110(4) 0.4477(3) 0.7859(4) 0.0242(13) Uani 1 1 d . . .
H11A H 0.4716 0.4265 0.8235 0.029 Uiso 1 1 calc R . .
H11B H 0.5642 0.4638 0.8319 0.029 Uiso 1 1 calc R . .
C12 C 0.5377(4) 0.3963(3) 0.7190(4) 0.0234(14) Uani 1 1 d . . .
C13 C 0.6191(4) 0.4044(3) 0.6929(4) 0.0290(15) Uani 1 1 d . . .
H13 H 0.6599 0.4368 0.7249 0.035 Uiso 1 1 calc R . .
C14 C 0.6408(5) 0.3652(3) 0.6200(5) 0.0351(17) Uani 1 1 d . . .
H14 H 0.6962 0.3708 0.6029 0.042 Uiso 1 1 calc R . .
C15 C 0.5821(4) 0.3188(3) 0.5735(5) 0.0321(16) Uani 1 1 d . . .
H15 H 0.5944 0.2950 0.5201 0.039 Uiso 1 1 calc R . .
C16 C 0.5037(4) 0.3062(3) 0.6047(4) 0.0278(15) Uani 1 1 d . . .
H16 H 0.4650 0.2719 0.5750 0.033 Uiso 1 1 calc R . .
C17 C 0.4821(4) 0.3440(3) 0.6797(4) 0.0206(13) Uani 1 1 d . . .
C18 C 0.4461(5) 0.2768(4) 0.8694(4) 0.0373(17) Uani 1 1 d . . .
H18A H 0.4082 0.2502 0.9019 0.056 Uiso 1 1 calc R . .
H18B H 0.4711 0.3143 0.9108 0.056 Uiso 1 1 calc R . .
H18C H 0.4940 0.2488 0.8566 0.056 Uiso 1 1 calc R . .
C19 C 0.3439(5) 0.2202(3) 0.6648(5) 0.0367(17) Uani 1 1 d . . .
H19A H 0.3221 0.2275 0.5955 0.055 Uiso 1 1 calc R . .
H19B H 0.2993 0.1960 0.6907 0.055 Uiso 1 1 calc R . .
H19C H 0.3985 0.1940 0.6755 0.055 Uiso 1 1 calc R . .
C20 C 0.0947(5) 0.2374(3) 0.6308(5) 0.0445(19) Uani 1 1 d . . .
H20A H 0.1239 0.2139 0.6896 0.067 Uiso 1 1 calc R . .
H20B H 0.1243 0.2265 0.5785 0.067 Uiso 1 1 calc R . .
H20C H 0.0327 0.2235 0.6126 0.067 Uiso 1 1 calc R . .
C21 C 0.0143(5) 0.3668(4) 0.5209(5) 0.0443(19) Uani 1 1 d . . .
H21A H 0.0424 0.3552 0.4676 0.066 Uiso 1 1 calc R . .
H21B H 0.0020 0.4148 0.5195 0.066 Uiso 1 1 calc R . .
H21C H -0.0411 0.3419 0.5141 0.066 Uiso 1 1 calc R . .
C22 C 0.0056(4) 0.3496(3) 0.7441(4) 0.0292(15) Uani 1 1 d . . .
C23 C -0.0157(4) 0.2918(3) 0.7905(5) 0.0379(17) Uani 1 1 d . . .
H23 H 0.0150 0.2513 0.7860 0.046 Uiso 1 1 calc R . .
C24 C -0.0817(5) 0.2940(4) 0.8428(6) 0.053(2) Uani 1 1 d . . .
H24 H -0.0944 0.2551 0.8757 0.063 Uiso 1 1 calc R . .
C25 C -0.1286(5) 0.3511(4) 0.8477(6) 0.054(2) Uani 1 1 d . . .
H25 H -0.1752 0.3515 0.8814 0.065 Uiso 1 1 calc R . .
C26 C -0.1076(5) 0.4082(4) 0.8033(5) 0.0426(19) Uani 1 1 d . . .
H26 H -0.1417 0.4475 0.8044 0.051 Uiso 1 1 calc R . .
C27 C -0.0363(4) 0.4094(4) 0.7562(5) 0.0327(16) Uani 1 1 d . . .
C28 C -0.0061(4) 0.4760(3) 0.7226(4) 0.0294(15) Uani 1 1 d . . .
H28A H 0.0211 0.4685 0.6666 0.035 Uiso 1 1 calc R . .
H28B H -0.0578 0.5056 0.7019 0.035 Uiso 1 1 calc R . .
C29 C 0.0138(4) 0.5374(3) 0.8741(4) 0.0317(16) Uani 1 1 d . . .
H29A H 0.0576 0.5584 0.9258 0.048 Uiso 1 1 calc R . .
H29B H -0.0168 0.5019 0.9012 0.048 Uiso 1 1 calc R . .
H29C H -0.0291 0.5710 0.8434 0.048 Uiso 1 1 calc R . .
C30 C 0.1046(4) 0.5618(3) 0.7610(4) 0.0276(15) Uani 1 1 d . . .
H30A H 0.0617 0.5967 0.7321 0.033 Uiso 1 1 calc R . .
H30B H 0.1316 0.5434 0.7095 0.033 Uiso 1 1 calc R . .
C31 C 0.1757(4) 0.5923(3) 0.8398(4) 0.0241(14) Uani 1 1 d . . .
C32 C 0.1815(4) 0.6614(3) 0.8488(5) 0.0296(15) Uani 1 1 d . . .
H32 H 0.1408 0.6884 0.8053 0.035 Uiso 1 1 calc R . .
C33 C 0.2447(4) 0.6915(3) 0.9192(5) 0.0284(15) Uani 1 1 d . . .
H33 H 0.2484 0.7388 0.9236 0.034 Uiso 1 1 calc R . .
C34 C 0.3028(4) 0.6520(3) 0.9834(5) 0.0317(16) Uani 1 1 d . . .
H34 H 0.3461 0.6721 1.0328 0.038 Uiso 1 1 calc R . .
C35 C 0.2980(4) 0.5826(3) 0.9758(4) 0.0268(14) Uani 1 1 d . . .
H35 H 0.3385 0.5561 1.0203 0.032 Uiso 1 1 calc R . .
C36 C 0.2351(4) 0.5514(3) 0.9044(4) 0.0237(14) Uani 1 1 d . . .
C37 C 0.3521(4) 0.4254(3) 0.9911(5) 0.0333(16) Uani 1 1 d . . .
H37A H 0.3463 0.4429 1.0538 0.050 Uiso 1 1 calc R . .
H37B H 0.4019 0.4471 0.9715 0.050 Uiso 1 1 calc R . .
H37C H 0.3623 0.3771 0.9960 0.050 Uiso 1 1 calc R . .
C38 C 0.1518(5) 0.4075(4) 0.9759(4) 0.0362(17) Uani 1 1 d . . .
H38A H 0.1577 0.4358 1.0331 0.054 Uiso 1 1 calc R . .
H38B H 0.1699 0.3618 0.9956 0.054 Uiso 1 1 calc R . .
H38C H 0.0902 0.4074 0.9402 0.054 Uiso 1 1 calc R . .
B1 B 0.2183(7) 0.3105(6) 0.3987(7) 0.056(3) Uani 1 1 d . . .
F1 F 0.2203(4) 0.2445(3) 0.3824(5) 0.107(2) Uani 1 1 d . . .
F2 F 0.2804(4) 0.3415(3) 0.3584(4) 0.0923(19) Uani 1 1 d . . .
F3 F 0.1360(4) 0.3384(3) 0.3524(4) 0.0869(18) Uani 1 1 d . . .
F4 F 0.2331(4) 0.3270(3) 0.4957(3) 0.0773(16) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0188(4) 0.0214(4) 0.0214(4) 0.0000(3) 0.0060(3) 0.0009(3)
Sb1 0.0244(2) 0.0194(2) 0.0199(2) 0.00172(16) 0.00529(17) 0.00277(17)
Sb2 0.0218(2) 0.0211(2) 0.0248(2) 0.00170(17) 0.00564(17) 0.00256(18)
Sb3 0.0195(2) 0.0298(3) 0.0321(2) -0.00832(19) 0.00620(18) -0.00172(19)
Sb4 0.0272(2) 0.0221(2) 0.0217(2) -0.00145(17) 0.00883(17) -0.00171(18)
N1 0.026(3) 0.020(3) 0.020(2) 0.001(2) 0.011(2) 0.001(2)
N2 0.023(3) 0.027(3) 0.024(3) -0.004(2) 0.011(2) -0.003(2)
C1 0.047(4) 0.026(4) 0.030(3) 0.000(3) 0.016(3) 0.008(3)
C2 0.036(4) 0.029(4) 0.041(4) 0.005(3) -0.013(3) 0.006(3)
C3 0.022(3) 0.020(3) 0.024(3) 0.001(3) 0.011(3) 0.000(3)
C4 0.024(4) 0.036(4) 0.027(3) 0.008(3) 0.012(3) 0.006(3)
C5 0.030(4) 0.024(4) 0.040(4) 0.009(3) 0.015(3) 0.008(3)
C6 0.038(4) 0.018(4) 0.053(4) -0.004(3) 0.031(4) 0.002(3)
C7 0.023(3) 0.026(4) 0.032(3) -0.001(3) 0.015(3) 0.001(3)
C8 0.021(3) 0.023(3) 0.027(3) 0.002(3) 0.015(3) 0.001(3)
C9 0.022(3) 0.024(3) 0.023(3) -0.006(3) 0.007(3) -0.003(3)
C10 0.030(4) 0.024(4) 0.045(4) 0.014(3) 0.021(3) 0.008(3)
C11 0.022(3) 0.021(3) 0.028(3) 0.000(3) 0.003(3) 0.001(3)
C12 0.021(3) 0.026(4) 0.026(3) 0.003(3) 0.011(3) 0.007(3)
C13 0.026(4) 0.023(4) 0.038(4) 0.002(3) 0.007(3) 0.005(3)
C14 0.036(4) 0.026(4) 0.047(4) 0.014(3) 0.018(3) 0.010(3)
C15 0.035(4) 0.030(4) 0.034(4) -0.002(3) 0.014(3) 0.013(3)
C16 0.033(4) 0.026(4) 0.027(3) 0.001(3) 0.011(3) 0.003(3)
C17 0.021(3) 0.014(3) 0.025(3) 0.005(2) 0.001(3) 0.004(3)
C18 0.038(4) 0.041(4) 0.031(4) 0.012(3) 0.003(3) 0.003(3)
C19 0.036(4) 0.024(4) 0.053(4) -0.005(3) 0.015(3) -0.001(3)
C20 0.045(5) 0.032(4) 0.057(5) -0.020(4) 0.011(4) 0.001(4)
C21 0.030(4) 0.065(6) 0.035(4) -0.017(4) 0.002(3) 0.000(4)
C22 0.018(3) 0.036(4) 0.034(3) -0.017(3) 0.007(3) -0.009(3)
C23 0.032(4) 0.020(4) 0.065(5) -0.004(3) 0.018(4) -0.012(3)
C24 0.050(5) 0.039(5) 0.080(6) -0.006(4) 0.038(5) -0.014(4)
C25 0.039(5) 0.042(5) 0.091(6) -0.016(5) 0.035(5) -0.012(4)
C26 0.028(4) 0.043(5) 0.060(5) -0.010(4) 0.015(4) -0.003(3)
C27 0.015(3) 0.042(4) 0.039(4) -0.012(3) 0.004(3) -0.009(3)
C28 0.028(4) 0.032(4) 0.028(3) -0.006(3) 0.006(3) 0.008(3)
C29 0.029(4) 0.038(4) 0.031(3) -0.009(3) 0.015(3) -0.003(3)
C30 0.027(4) 0.030(4) 0.027(3) 0.006(3) 0.007(3) 0.006(3)
C31 0.023(3) 0.031(4) 0.020(3) -0.003(3) 0.008(3) 0.001(3)
C32 0.034(4) 0.027(4) 0.032(4) 0.000(3) 0.018(3) -0.002(3)
C33 0.032(4) 0.017(3) 0.040(4) -0.003(3) 0.016(3) 0.000(3)
C34 0.028(4) 0.031(4) 0.036(4) -0.014(3) 0.009(3) -0.009(3)
C35 0.024(4) 0.030(4) 0.026(3) -0.001(3) 0.006(3) 0.006(3)
C36 0.022(3) 0.023(3) 0.028(3) -0.005(3) 0.010(3) 0.000(3)
C37 0.032(4) 0.027(4) 0.041(4) -0.001(3) 0.008(3) 0.005(3)
C38 0.044(4) 0.040(4) 0.029(4) 0.016(3) 0.019(3) 0.008(3)
B1 0.054(7) 0.073(8) 0.041(5) -0.024(5) 0.016(5) -0.003(6)
F1 0.118(5) 0.052(4) 0.163(6) -0.045(4) 0.055(5) -0.010(4)
F2 0.095(4) 0.114(5) 0.084(4) -0.027(4) 0.055(4) -0.023(4)
F3 0.080(4) 0.104(5) 0.076(4) -0.034(3) 0.013(3) 0.014(3)
F4 0.105(4) 0.081(4) 0.051(3) -0.001(3) 0.028(3) 0.020(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Sb3 2.5289(9) . ?
Cu1 Sb1 2.5291(8) . ?
Cu1 Sb2 2.5317(9) . ?
Cu1 Sb4 2.5380(8) . ?
Sb1 C1 2.123(6) . ?
Sb1 C2 2.135(6) . ?
Sb1 C3 2.154(6) . ?
Sb2 C19 2.135(6) . ?
Sb2 C18 2.140(6) . ?
Sb2 C17 2.158(6) . ?
Sb3 C20 2.110(7) . ?
Sb3 C22 2.151(6) . ?
Sb3 C21 2.152(7) . ?
Sb4 C38 2.121(6) . ?
Sb4 C37 2.136(6) . ?
Sb4 C36 2.147(6) . ?
N1 C11 1.464(7) . ?
N1 C9 1.471(7) . ?
N1 C10 1.474(7) . ?
N2 C30 1.465(8) . ?
N2 C29 1.486(7) . ?
N2 C28 1.485(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.392(8) . ?
C3 C8 1.404(8) . ?
C4 C5 1.397(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.378(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.398(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.497(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.519(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C17 1.394(8) . ?
C12 C13 1.402(8) . ?
C13 C14 1.398(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.367(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.406(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.406(8) . ?
C16 H16 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C27 1.391(9) . ?
C22 C23 1.408(9) . ?
C23 C24 1.391(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.368(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.380(10) . ?
C25 H25 0.9500 . ?
C26 C27 1.413(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.525(9) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.519(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.392(9) . ?
C31 C36 1.412(8) . ?
C32 C33 1.379(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.383(9) . ?
C33 H33 0.9500 . ?
C34 C35 1.395(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.394(8) . ?
C35 H35 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
B1 F1 1.345(12) . ?
B1 F2 1.372(11) . ?
B1 F4 1.387(10) . ?
B1 F3 1.418(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Sb3 Cu1 Sb1 111.05(3) . . ?
Sb3 Cu1 Sb2 108.42(3) . . ?
Sb1 Cu1 Sb2 102.97(3) . . ?
Sb3 Cu1 Sb4 105.82(3) . . ?
Sb1 Cu1 Sb4 115.61(3) . . ?
Sb2 Cu1 Sb4 112.89(3) . . ?
C1 Sb1 C2 94.5(3) . . ?
C1 Sb1 C3 103.3(2) . . ?
C2 Sb1 C3 97.6(2) . . ?
C1 Sb1 Cu1 125.99(18) . . ?
C2 Sb1 Cu1 110.4(2) . . ?
C3 Sb1 Cu1 118.92(14) . . ?
C19 Sb2 C18 97.0(3) . . ?
C19 Sb2 C17 98.7(2) . . ?
C18 Sb2 C17 95.1(2) . . ?
C19 Sb2 Cu1 119.88(19) . . ?
C18 Sb2 Cu1 124.16(19) . . ?
C17 Sb2 Cu1 116.54(15) . . ?
C20 Sb3 C22 99.2(3) . . ?
C20 Sb3 C21 95.0(3) . . ?
C22 Sb3 C21 97.0(3) . . ?
C20 Sb3 Cu1 121.5(2) . . ?
C22 Sb3 Cu1 114.38(16) . . ?
C21 Sb3 Cu1 124.4(2) . . ?
C38 Sb4 C37 93.0(3) . . ?
C38 Sb4 C36 105.8(2) . . ?
C37 Sb4 C36 96.5(2) . . ?
C38 Sb4 Cu1 126.4(2) . . ?
C37 Sb4 Cu1 109.91(17) . . ?
C36 Sb4 Cu1 118.05(15) . . ?
C11 N1 C9 111.1(4) . . ?
C11 N1 C10 111.5(5) . . ?
C9 N1 C10 108.9(5) . . ?
C30 N2 C29 109.4(5) . . ?
C30 N2 C28 109.4(5) . . ?
C29 N2 C28 110.5(5) . . ?
Sb1 C1 H1A 109.5 . . ?
Sb1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Sb1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Sb1 C2 H2A 109.5 . . ?
Sb1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Sb1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 119.3(6) . . ?
C4 C3 Sb1 120.0(5) . . ?
C8 C3 Sb1 120.6(4) . . ?
C3 C4 C5 120.4(6) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 120.2(6) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 120.0(6) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C8 121.1(6) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C3 119.0(6) . . ?
C7 C8 C9 120.2(6) . . ?
C3 C8 C9 120.7(5) . . ?
N1 C9 C8 111.3(4) . . ?
N1 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
N1 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 111.1(5) . . ?
N1 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
N1 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C17 C12 C13 119.8(5) . . ?
C17 C12 C11 122.0(5) . . ?
C13 C12 C11 118.1(6) . . ?
C12 C13 C14 120.4(6) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 119.9(6) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.0(6) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C17 C16 C15 120.5(6) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C12 C17 C16 118.6(5) . . ?
C12 C17 Sb2 122.6(4) . . ?
C16 C17 Sb2 118.6(4) . . ?
Sb2 C18 H18A 109.5 . . ?
Sb2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Sb2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Sb2 C19 H19A 109.5 . . ?
Sb2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Sb2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Sb3 C20 H20A 109.5 . . ?
Sb3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Sb3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Sb3 C21 H21A 109.5 . . ?
Sb3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Sb3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C22 C23 119.2(6) . . ?
C27 C22 Sb3 122.7(5) . . ?
C23 C22 Sb3 118.1(5) . . ?
C24 C23 C22 120.0(7) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 121.0(7) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C24 C25 C26 119.4(7) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C25 C26 C27 121.2(7) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C22 C27 C26 118.6(6) . . ?
C22 C27 C28 122.1(5) . . ?
C26 C27 C28 119.2(6) . . ?
N2 C28 C27 110.7(5) . . ?
N2 C28 H28A 109.5 . . ?
C27 C28 H28A 109.5 . . ?
N2 C28 H28B 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
N2 C29 H29A 109.5 . . ?
N2 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N2 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N2 C30 C31 109.8(5) . . ?
N2 C30 H30A 109.7 . . ?
C31 C30 H30A 109.7 . . ?
N2 C30 H30B 109.7 . . ?
C31 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
C32 C31 C36 119.9(6) . . ?
C32 C31 C30 119.3(6) . . ?
C36 C31 C30 120.9(6) . . ?
C33 C32 C31 121.6(6) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C32 C33 C34 119.1(6) . . ?
C32 C33 H33 120.5 . . ?
C34 C33 H33 120.5 . . ?
C33 C34 C35 120.3(6) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C36 C35 C34 121.4(6) . . ?
C36 C35 H35 119.3 . . ?
C34 C35 H35 119.3 . . ?
C35 C36 C31 117.8(6) . . ?
C35 C36 Sb4 121.4(5) . . ?
C31 C36 Sb4 120.6(4) . . ?
Sb4 C37 H37A 109.5 . . ?
Sb4 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Sb4 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Sb4 C38 H38A 109.5 . . ?
Sb4 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Sb4 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
F1 B1 F2 109.2(7) . . ?
F1 B1 F4 113.7(9) . . ?
F2 B1 F4 109.2(8) . . ?
F1 B1 F3 111.1(8) . . ?
F2 B1 F3 105.7(9) . . ?
F4 B1 F3 107.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.174

#===END OF CIF ==============================================================
# 08mj48

data_08mj48
_database_code_depnum_ccdc_archive 'CCDC 731687'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2009-01-08
_audit_author_name               'Webster, M.'

_chemical_name_systematic        
;
tetracarbonyl-(bis(N-(2-(dimethylstibanyl)benzyl))-methanamine-Sb,Sb')-
molybdenum
;

# iLab IUPAC name of ligand:
# N-[2-(dimethylstibino)benzyl]-1-[2-(dimethylstibino)phenyl]-
# N-methylmethanamine
#
# How about bis(N-(2-(dimethylstibanyl)benzyl))-methanamine

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H27 Mo N O4 Sb2'
_chemical_formula_sum            'C23 H27 Mo N O4 Sb2'
_chemical_formula_structural     'Mo (C O)4 (C19 H27 N Sb2)'
_chemical_formula_weight         720.90

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.9439(10)
_cell_length_b                   7.1462(10)
_cell_length_c                   36.806(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.694(5)
_cell_angle_gamma                90.00
_cell_volume                     2591.9(6) # shelxl (5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    58186
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    2.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5824 # 0.7146
_exptl_absorpt_correction_T_max  0.7456 # 0.9041
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21865
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.82
_reflns_number_total             5554
_reflns_number_gt                5189
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+16.9072P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5554
_refine_ls_number_parameters     285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1043
_refine_ls_wR_factor_gt          0.1006
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.34251(4) 0.51986(6) 0.379797(11) 0.01638(11) Uani 1 1 d . . .
Sb1 Sb 0.13635(3) 0.39911(4) 0.326454(8) 0.01627(10) Uani 1 1 d . . .
Sb2 Sb 0.23437(3) 0.36142(5) 0.437541(9) 0.01840(10) Uani 1 1 d . . .
N1 N -0.1010(4) 0.4982(6) 0.36746(11) 0.0162(8) Uani 1 1 d . . .
O1 O 0.5842(4) 0.6496(6) 0.43736(12) 0.0332(10) Uani 1 1 d . . .
O2 O 0.4774(5) 0.7094(7) 0.31676(13) 0.0414(11) Uani 1 1 d . . .
O3 O 0.4916(4) 0.1354(6) 0.36686(15) 0.0411(11) Uani 1 1 d . . .
O4 O 0.2237(4) 0.9245(6) 0.39189(12) 0.0335(10) Uani 1 1 d . . .
C1 C 0.2342(6) 0.3015(9) 0.28151(15) 0.0305(13) Uani 1 1 d . . .
H1A H 0.3045 0.2102 0.2905 0.046 Uiso 1 1 calc R . .
H1B H 0.2759 0.4075 0.2703 0.046 Uiso 1 1 calc R . .
H1C H 0.1670 0.2421 0.2632 0.046 Uiso 1 1 calc R . .
C2 C 0.0242(6) 0.1476(7) 0.32958(17) 0.0272(12) Uani 1 1 d . . .
H2A H -0.0038 0.1366 0.3540 0.041 Uiso 1 1 calc R . .
H2B H 0.0812 0.0403 0.3251 0.041 Uiso 1 1 calc R . .
H2C H -0.0563 0.1500 0.3111 0.041 Uiso 1 1 calc R . .
C3 C -0.0055(5) 0.5856(7) 0.29582(13) 0.0162(9) Uani 1 1 d . . .
C4 C -0.0036(5) 0.6011(8) 0.25812(14) 0.0221(11) Uani 1 1 d . . .
H4 H 0.0591 0.5287 0.2467 0.027 Uiso 1 1 calc R . .
C5 C -0.0924(5) 0.7217(8) 0.23695(14) 0.0259(11) Uani 1 1 d . . .
H5 H -0.0892 0.7326 0.2114 0.031 Uiso 1 1 calc R . .
C6 C -0.1844(5) 0.8243(8) 0.25318(15) 0.0247(11) Uani 1 1 d . . .
H6 H -0.2451 0.9063 0.2388 0.030 Uiso 1 1 calc R . .
C7 C -0.1893(5) 0.8086(7) 0.29064(14) 0.0202(10) Uani 1 1 d . . .
H7 H -0.2557 0.8766 0.3015 0.024 Uiso 1 1 calc R . .
C8 C -0.0980(5) 0.6943(6) 0.31245(14) 0.0168(9) Uani 1 1 d . . .
C9 C -0.0993(5) 0.6896(7) 0.35358(14) 0.0190(10) Uani 1 1 d . . .
H9A H -0.0179 0.7551 0.3659 0.023 Uiso 1 1 calc R . .
H9B H -0.1804 0.7571 0.3596 0.023 Uiso 1 1 calc R . .
C10 C -0.2267(5) 0.4069(8) 0.35251(14) 0.0212(10) Uani 1 1 d . . .
H10A H -0.3035 0.4731 0.3607 0.032 Uiso 1 1 calc R . .
H10B H -0.2257 0.2769 0.3610 0.032 Uiso 1 1 calc R . .
H10C H -0.2358 0.4090 0.3257 0.032 Uiso 1 1 calc R . .
C11 C -0.0881(5) 0.5061(7) 0.40811(13) 0.0182(10) Uani 1 1 d . . .
H11A H -0.1670 0.5743 0.4153 0.022 Uiso 1 1 calc R . .
H11B H -0.0053 0.5774 0.4175 0.022 Uiso 1 1 calc R . .
C12 C -0.0805(5) 0.3141(7) 0.42579(13) 0.0189(10) Uani 1 1 d . . .
C13 C -0.2032(6) 0.2262(8) 0.43025(14) 0.0249(11) Uani 1 1 d . . .
H13 H -0.2865 0.2907 0.4237 0.030 Uiso 1 1 calc R . .
C14 C -0.2039(6) 0.0448(8) 0.44421(15) 0.0285(12) Uani 1 1 d . . .
H14 H -0.2877 -0.0156 0.4462 0.034 Uiso 1 1 calc R . .
C15 C -0.0825(6) -0.0476(8) 0.45521(16) 0.0296(12) Uani 1 1 d . . .
H15 H -0.0826 -0.1714 0.4646 0.035 Uiso 1 1 calc R . .
C16 C 0.0390(6) 0.0429(7) 0.45227(15) 0.0254(11) Uani 1 1 d . . .
H16 H 0.1220 -0.0192 0.4605 0.030 Uiso 1 1 calc R . .
C17 C 0.0426(5) 0.2222(7) 0.43766(13) 0.0184(10) Uani 1 1 d . . .
C18 C 0.2191(6) 0.5471(8) 0.48251(15) 0.0302(13) Uani 1 1 d . . .
H18A H 0.1423 0.6323 0.4761 0.045 Uiso 1 1 calc R . .
H18B H 0.3030 0.6198 0.4877 0.045 Uiso 1 1 calc R . .
H18C H 0.2049 0.4742 0.5042 0.045 Uiso 1 1 calc R . .
C19 C 0.3677(6) 0.1627(9) 0.46750(16) 0.0314(13) Uani 1 1 d . . .
H19A H 0.4585 0.2172 0.4731 0.047 Uiso 1 1 calc R . .
H19B H 0.3724 0.0494 0.4527 0.047 Uiso 1 1 calc R . .
H19C H 0.3330 0.1305 0.4904 0.047 Uiso 1 1 calc R . .
C20 C 0.4960(5) 0.5996(7) 0.41623(15) 0.0226(11) Uani 1 1 d . . .
C21 C 0.4281(6) 0.6381(8) 0.33963(16) 0.0268(12) Uani 1 1 d . . .
C22 C 0.4366(5) 0.2695(8) 0.37127(15) 0.0244(11) Uani 1 1 d . . .
C23 C 0.2601(5) 0.7738(8) 0.38751(14) 0.0219(10) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0123(2) 0.0188(2) 0.0174(2) 0.00079(16) -0.00035(16) -0.00096(15)
Sb1 0.01402(16) 0.01797(16) 0.01601(16) -0.00087(12) -0.00092(12) 0.00153(11)
Sb2 0.01753(17) 0.02089(17) 0.01597(16) 0.00184(13) -0.00075(13) 0.00015(12)
N1 0.0160(19) 0.0179(19) 0.0145(18) -0.0012(16) 0.0010(16) -0.0042(16)
O1 0.0216(19) 0.037(2) 0.037(2) -0.0062(19) -0.0076(17) -0.0037(17)
O2 0.038(2) 0.052(3) 0.036(2) 0.013(2) 0.011(2) -0.005(2)
O3 0.028(2) 0.029(2) 0.067(3) -0.008(2) 0.006(2) 0.0064(18)
O4 0.032(2) 0.024(2) 0.043(2) -0.0068(19) 0.0040(19) 0.0030(17)
C1 0.029(3) 0.041(3) 0.022(3) -0.008(2) 0.005(2) 0.012(3)
C2 0.028(3) 0.013(2) 0.040(3) -0.002(2) 0.002(2) -0.003(2)
C3 0.015(2) 0.017(2) 0.015(2) 0.0059(18) -0.0027(18) -0.0018(18)
C4 0.019(2) 0.028(3) 0.019(2) 0.005(2) 0.000(2) 0.001(2)
C5 0.025(3) 0.035(3) 0.017(2) 0.010(2) 0.000(2) 0.000(2)
C6 0.022(3) 0.025(3) 0.026(3) 0.004(2) -0.003(2) 0.003(2)
C7 0.019(2) 0.019(2) 0.023(2) 0.001(2) 0.003(2) 0.0012(19)
C8 0.014(2) 0.014(2) 0.021(2) 0.0011(19) -0.0016(19) -0.0035(17)
C9 0.018(2) 0.018(2) 0.020(2) -0.0003(19) 0.0015(19) -0.0007(19)
C10 0.016(2) 0.029(3) 0.019(2) 0.004(2) 0.0018(19) -0.008(2)
C11 0.019(2) 0.020(2) 0.016(2) -0.0031(19) 0.0010(19) 0.0003(19)
C12 0.023(2) 0.023(2) 0.012(2) -0.0007(19) 0.0049(19) -0.003(2)
C13 0.025(3) 0.032(3) 0.019(2) -0.002(2) 0.006(2) -0.003(2)
C14 0.034(3) 0.033(3) 0.020(2) -0.006(2) 0.009(2) -0.012(2)
C15 0.042(3) 0.023(3) 0.026(3) -0.003(2) 0.010(3) -0.008(2)
C16 0.035(3) 0.020(2) 0.022(2) 0.004(2) 0.005(2) 0.000(2)
C17 0.022(2) 0.019(2) 0.015(2) 0.0001(19) 0.0046(19) -0.0023(19)
C18 0.037(3) 0.030(3) 0.023(3) -0.004(2) 0.000(2) -0.004(2)
C19 0.029(3) 0.035(3) 0.028(3) 0.007(2) -0.003(2) 0.008(2)
C20 0.017(2) 0.023(2) 0.028(3) 0.002(2) 0.002(2) 0.0022(19)
C21 0.020(2) 0.032(3) 0.028(3) 0.005(2) 0.002(2) 0.000(2)
C22 0.017(2) 0.026(3) 0.029(3) -0.003(2) 0.002(2) -0.001(2)
C23 0.017(2) 0.027(3) 0.022(2) -0.001(2) 0.002(2) -0.005(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C20 1.976(5) . ?
Mo1 C21 1.991(6) . ?
Mo1 C23 2.027(6) . ?
Mo1 C22 2.063(6) . ?
Mo1 Sb2 2.7509(6) . ?
Mo1 Sb1 2.7792(5) . ?
Sb1 C2 2.126(5) . ?
Sb1 C1 2.145(5) . ?
Sb1 C3 2.147(4) . ?
Sb2 C18 2.143(6) . ?
Sb2 C19 2.145(5) . ?
Sb2 C17 2.151(5) . ?
N1 C10 1.452(6) . ?
N1 C9 1.461(6) . ?
N1 C11 1.486(6) . ?
O1 C20 1.149(6) . ?
O2 C21 1.148(7) . ?
O3 C22 1.126(7) . ?
O4 C23 1.154(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.395(7) . ?
C3 C8 1.405(7) . ?
C4 C5 1.395(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.370(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.391(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.393(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.516(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.516(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.401(7) . ?
C12 C17 1.407(7) . ?
C13 C14 1.395(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.388(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.392(7) . ?
C16 H16 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C20 Mo1 C21 90.8(2) . . ?
C20 Mo1 C23 86.4(2) . . ?
C21 Mo1 C23 86.9(2) . . ?
C20 Mo1 C22 91.6(2) . . ?
C21 Mo1 C22 90.4(2) . . ?
C23 Mo1 C22 176.6(2) . . ?
C20 Mo1 Sb2 86.60(16) . . ?
C21 Mo1 Sb2 177.36(16) . . ?
C23 Mo1 Sb2 93.04(15) . . ?
C22 Mo1 Sb2 89.58(16) . . ?
C20 Mo1 Sb1 177.01(16) . . ?
C21 Mo1 Sb1 87.45(16) . . ?
C23 Mo1 Sb1 95.91(14) . . ?
C22 Mo1 Sb1 85.97(14) . . ?
Sb2 Mo1 Sb1 95.183(18) . . ?
C2 Sb1 C1 93.6(2) . . ?
C2 Sb1 C3 103.9(2) . . ?
C1 Sb1 C3 97.5(2) . . ?
C2 Sb1 Mo1 124.52(16) . . ?
C1 Sb1 Mo1 106.13(16) . . ?
C3 Sb1 Mo1 123.28(13) . . ?
C18 Sb2 C19 96.7(2) . . ?
C18 Sb2 C17 97.5(2) . . ?
C19 Sb2 C17 100.4(2) . . ?
C18 Sb2 Mo1 114.66(17) . . ?
C19 Sb2 Mo1 113.03(17) . . ?
C17 Sb2 Mo1 129.06(13) . . ?
C10 N1 C9 109.8(4) . . ?
C10 N1 C11 110.6(4) . . ?
C9 N1 C11 108.2(4) . . ?
Sb1 C1 H1A 109.5 . . ?
Sb1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Sb1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Sb1 C2 H2A 109.5 . . ?
Sb1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Sb1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 119.1(4) . . ?
C4 C3 Sb1 118.4(4) . . ?
C8 C3 Sb1 122.5(3) . . ?
C5 C4 C3 120.8(5) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C6 C5 C4 119.8(5) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.2(5) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 120.8(5) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C7 C8 C3 119.2(5) . . ?
C7 C8 C9 119.7(5) . . ?
C3 C8 C9 121.1(4) . . ?
N1 C9 C8 111.8(4) . . ?
N1 C9 H9A 109.3 . . ?
C8 C9 H9A 109.3 . . ?
N1 C9 H9B 109.3 . . ?
C8 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 113.0(4) . . ?
N1 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
N1 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C13 C12 C17 119.3(5) . . ?
C13 C12 C11 117.5(5) . . ?
C17 C12 C11 123.2(5) . . ?
C14 C13 C12 120.4(5) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 120.2(5) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 119.2(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 121.8(5) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C16 C17 C12 118.9(5) . . ?
C16 C17 Sb2 119.7(4) . . ?
C12 C17 Sb2 121.2(4) . . ?
Sb2 C18 H18A 109.5 . . ?
Sb2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Sb2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Sb2 C19 H19A 109.5 . . ?
Sb2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Sb2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C20 Mo1 178.6(5) . . ?
O2 C21 Mo1 178.8(6) . . ?
O3 C22 Mo1 177.9(5) . . ?
O4 C23 Mo1 174.3(5) . . ?

_diffrn_measured_fraction_theta_max 0.906
_diffrn_reflns_theta_full        27.82
_diffrn_measured_fraction_theta_full 0.906
_refine_diff_density_max         1.284
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.216

#===END OF CIF ==============================================================
# 08mj47

data_08mj47
_database_code_depnum_ccdc_archive 'CCDC 731688'

_audit_creation_method           'SHELXL-97 + hand edit'
_audit_creation_date             2009-01-09
_audit_author_name               'Webster, M.'

_chemical_name_systematic        
;
Iodotrimethyl-(bis(N-(2-(dimethylstibanyl)benzyl))-methanamine-Sb,Sb')-
platinum
;

# iLab IUPAC name of ligand:
# N-[2-(dimethylstibino)benzyl]-1-[2-(dimethylstibino)phenyl]-
# N-methylmethanamine
#
# bis(N-(2-(dimethylstibanyl)benzyl))-methanamine

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H36 I N Pt Sb2'
_chemical_formula_sum            'C22 H36 I N Pt Sb2'
_chemical_formula_structural     'Pt I (C H3)3 (C19 H27 N Sb2)'
_chemical_formula_weight         880.01

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'
N N 0.0061 0.0033 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.843(4)
_cell_length_b                   10.645(3)
_cell_length_c                   15.405(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.431(15)
_cell_angle_gamma                90.00
_cell_volume                     2588.2(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    36291
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    8.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4921 #
_exptl_absorpt_correction_T_max  0.7456 #
_exptl_absorpt_process_details   
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29377
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         27.54
_reflns_number_total             5919
_reflns_number_gt                4588
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+4.7266P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5919
_refine_ls_number_parameters     252
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.1041
_refine_ls_wR_factor_gt          0.0948
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.231628(18) 0.39966(2) 0.336373(18) 0.02256(10) Uani 1 1 d . . .
I1 I 0.20141(3) 0.44952(5) 0.50041(3) 0.03337(14) Uani 1 1 d . . .
Sb1 Sb 0.35857(3) 0.25949(4) 0.43865(3) 0.02511(13) Uani 1 1 d . . .
Sb2 Sb 0.11385(3) 0.22868(4) 0.30050(4) 0.02689(13) Uani 1 1 d . . .
N1 N 0.3217(5) 0.0216(6) 0.3377(4) 0.0353(16) Uani 1 1 d . . .
C1 C 0.4358(4) 0.3831(6) 0.5405(5) 0.0199(14) Uani 1 1 d . . .
H1A H 0.4124 0.3926 0.5902 0.030 Uiso 1 1 calc R . .
H1B H 0.4374 0.4652 0.5125 0.030 Uiso 1 1 calc RD . .
H1C H 0.4933 0.3488 0.5661 0.030 Uiso 1 1 calc R . .
C2 C 0.3532(6) 0.1308(8) 0.5419(6) 0.040(2) Uani 1 1 d . . .
H2A H 0.4081 0.0889 0.5692 0.060 Uiso 1 1 calc R . .
H2B H 0.3092 0.0678 0.5139 0.060 Uiso 1 1 calc R . .
H2C H 0.3397 0.1762 0.5904 0.060 Uiso 1 1 calc R . .
C3 C 0.4565(5) 0.2111(7) 0.3847(5) 0.0280(16) Uani 1 1 d . . .
C4 C 0.5328(5) 0.2745(7) 0.4178(5) 0.0308(17) Uani 1 1 d . . .
H4 H 0.5412 0.3358 0.4651 0.037 Uiso 1 1 calc R . .
C5 C 0.5975(6) 0.2506(8) 0.3834(7) 0.041(2) Uani 1 1 d . . .
H5 H 0.6495 0.2954 0.4070 0.049 Uiso 1 1 calc R . .
C6 C 0.5862(6) 0.1630(9) 0.3161(7) 0.050(2) Uani 1 1 d . . .
H6 H 0.6304 0.1460 0.2928 0.060 Uiso 1 1 calc R . .
C7 C 0.5091(6) 0.0976(9) 0.2810(6) 0.045(2) Uani 1 1 d . . .
H7 H 0.5020 0.0348 0.2351 0.054 Uiso 1 1 calc R . .
C8 C 0.4429(5) 0.1241(7) 0.3131(5) 0.0292(17) Uani 1 1 d . . .
C9 C 0.3583(5) 0.0592(8) 0.2699(5) 0.0344(18) Uani 1 1 d . . .
H9A H 0.3186 0.1166 0.2247 0.041 Uiso 1 1 calc R . .
H9B H 0.3658 -0.0161 0.2358 0.041 Uiso 1 1 calc R . .
C10 C 0.3751(6) -0.0794(8) 0.3974(6) 0.041(2) Uani 1 1 d . . .
H10A H 0.3786 -0.1507 0.3587 0.061 Uiso 1 1 calc R . .
H10B H 0.3497 -0.1070 0.4425 0.061 Uiso 1 1 calc R . .
H10C H 0.4322 -0.0468 0.4303 0.061 Uiso 1 1 calc R . .
C11 C 0.2341(5) -0.0246(8) 0.2920(6) 0.0367(19) Uani 1 1 d . . .
H11A H 0.2363 -0.1058 0.2615 0.044 Uiso 1 1 calc R . .
H11B H 0.2031 0.0358 0.2430 0.044 Uiso 1 1 calc R . .
C12 C 0.1854(5) -0.0425(7) 0.3568(5) 0.0290(16) Uani 1 1 d . . .
C13 C 0.1922(5) -0.1547(7) 0.4056(6) 0.0374(19) Uani 1 1 d . . .
H13 H 0.2230 -0.2225 0.3926 0.045 Uiso 1 1 calc R . .
C14 C 0.1552(6) -0.1703(8) 0.4728(6) 0.043(2) Uani 1 1 d . . .
H14 H 0.1619 -0.2471 0.5061 0.052 Uiso 1 1 calc R . .
C15 C 0.1088(6) -0.0736(8) 0.4906(6) 0.040(2) Uani 1 1 d . . .
H15 H 0.0838 -0.0832 0.5367 0.047 Uiso 1 1 calc R . .
C16 C 0.0985(5) 0.0379(7) 0.4414(6) 0.0344(18) Uani 1 1 d . . .
H16 H 0.0661 0.1041 0.4537 0.041 Uiso 1 1 calc R . .
C17 C 0.1354(5) 0.0539(7) 0.3739(5) 0.0275(16) Uani 1 1 d . . .
C18 C 0.0037(5) 0.2927(8) 0.3248(7) 0.041(2) Uani 1 1 d . . .
H18A H -0.0352 0.2221 0.3189 0.061 Uiso 1 1 calc R . .
H18B H -0.0244 0.3575 0.2793 0.061 Uiso 1 1 calc R . .
H18C H 0.0200 0.3279 0.3873 0.061 Uiso 1 1 calc R . .
C19 C 0.0550(5) 0.1732(8) 0.1579(5) 0.0377(19) Uani 1 1 d . . .
H19A H 0.0268 0.0919 0.1548 0.057 Uiso 1 1 calc R . .
H19B H 0.0982 0.1661 0.1290 0.057 Uiso 1 1 calc R . .
H19C H 0.0130 0.2365 0.1248 0.057 Uiso 1 1 calc R . .
C20 C 0.2566(5) 0.3742(7) 0.2128(5) 0.0323(18) Uani 1 1 d . . .
H20A H 0.2216 0.3055 0.1770 0.048 Uiso 1 1 calc R . .
H20B H 0.3166 0.3535 0.2277 0.048 Uiso 1 1 calc R . .
H20C H 0.2434 0.4518 0.1763 0.048 Uiso 1 1 calc R . .
C21 C 0.1377(5) 0.5260(7) 0.2616(5) 0.0345(18) Uani 1 1 d . . .
H21A H 0.1193 0.5759 0.3045 0.052 Uiso 1 1 calc R . .
H21B H 0.0894 0.4795 0.2196 0.052 Uiso 1 1 calc R . .
H21C H 0.1606 0.5820 0.2255 0.052 Uiso 1 1 calc R . .
C22 C 0.3166(5) 0.5497(7) 0.3587(6) 0.0316(17) Uani 1 1 d . . .
H22A H 0.2974 0.6074 0.3059 0.047 Uiso 1 1 calc R . .
H22B H 0.3730 0.5177 0.3655 0.047 Uiso 1 1 calc R . .
H22C H 0.3192 0.5945 0.4153 0.047 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.02086(17) 0.02078(15) 0.02583(16) 0.00104(10) 0.00786(12) 0.00107(11)
I1 0.0359(3) 0.0345(3) 0.0323(3) -0.0021(2) 0.0150(2) 0.0030(2)
Sb1 0.0213(3) 0.0291(3) 0.0244(3) 0.00162(18) 0.0074(2) 0.0047(2)
Sb2 0.0215(3) 0.0224(2) 0.0343(3) -0.00138(19) 0.0066(2) -0.00074(19)
N1 0.036(4) 0.045(4) 0.021(3) 0.000(3) 0.005(3) 0.015(3)
C1 0.006(3) 0.015(3) 0.038(4) -0.008(3) 0.006(3) -0.001(2)
C2 0.043(6) 0.043(5) 0.038(5) 0.008(4) 0.021(4) 0.012(4)
C3 0.026(4) 0.029(4) 0.032(4) 0.004(3) 0.014(3) 0.004(3)
C4 0.023(4) 0.035(4) 0.032(4) 0.004(3) 0.008(3) 0.006(3)
C5 0.027(5) 0.045(5) 0.057(6) 0.016(4) 0.023(4) 0.003(4)
C6 0.038(6) 0.055(6) 0.069(7) 0.004(5) 0.034(5) 0.011(5)
C7 0.045(6) 0.059(6) 0.037(5) 0.000(4) 0.023(4) 0.015(5)
C8 0.029(5) 0.033(4) 0.027(4) 0.000(3) 0.011(3) 0.006(3)
C9 0.032(5) 0.037(4) 0.033(4) -0.007(3) 0.011(4) 0.008(4)
C10 0.027(5) 0.038(5) 0.050(5) 0.011(4) 0.004(4) 0.008(4)
C11 0.030(5) 0.037(4) 0.038(5) -0.007(3) 0.005(4) 0.006(4)
C12 0.012(4) 0.030(4) 0.034(4) -0.001(3) -0.006(3) 0.003(3)
C13 0.022(4) 0.028(4) 0.052(5) 0.001(4) 0.001(4) 0.009(3)
C14 0.033(5) 0.037(5) 0.053(5) 0.015(4) 0.008(4) -0.009(4)
C15 0.030(5) 0.047(5) 0.043(5) 0.001(4) 0.013(4) -0.010(4)
C16 0.027(5) 0.028(4) 0.047(5) 0.000(3) 0.011(4) 0.002(3)
C17 0.026(4) 0.023(4) 0.026(4) -0.003(3) 0.000(3) -0.005(3)
C18 0.025(5) 0.033(4) 0.069(6) -0.002(4) 0.020(4) 0.000(4)
C19 0.026(5) 0.039(5) 0.040(5) -0.004(4) 0.002(4) 0.002(4)
C20 0.033(5) 0.034(4) 0.036(4) 0.008(3) 0.021(4) 0.004(3)
C21 0.032(5) 0.039(4) 0.034(4) 0.008(3) 0.014(4) 0.010(4)
C22 0.025(4) 0.024(4) 0.044(5) 0.000(3) 0.009(4) 0.002(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C21 2.090(8) . ?
Pt1 C22 2.092(7) . ?
Pt1 C20 2.105(7) . ?
Pt1 Sb2 2.6053(7) . ?
Pt1 Sb1 2.6321(7) . ?
Pt1 I1 2.7972(7) . ?
Sb1 C1 2.112(6) . ?
Sb1 C2 2.126(8) . ?
Sb1 C3 2.153(7) . ?
Sb2 C18 2.128(8) . ?
Sb2 C17 2.142(7) . ?
Sb2 C19 2.154(8) . ?
N1 C9 1.442(10) . ?
N1 C11 1.480(11) . ?
N1 C10 1.495(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.381(11) . ?
C3 C8 1.397(10) . ?
C4 C5 1.393(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.357(13) . ?
C5 H5 0.9500 . ?
C6 C7 1.404(14) . ?
C6 H6 0.9500 . ?
C7 C8 1.398(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.513(12) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.510(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.395(11) . ?
C12 C17 1.409(10) . ?
C13 C14 1.392(12) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(13) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.395(11) . ?
C16 H16 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 Pt1 C22 86.7(3) . . ?
C21 Pt1 C20 86.3(3) . . ?
C22 Pt1 C20 84.6(3) . . ?
C21 Pt1 Sb2 87.7(2) . . ?
C22 Pt1 Sb2 174.3(2) . . ?
C20 Pt1 Sb2 95.5(2) . . ?
C21 Pt1 Sb1 174.4(2) . . ?
C22 Pt1 Sb1 88.2(2) . . ?
C20 Pt1 Sb1 95.2(2) . . ?
Sb2 Pt1 Sb1 97.48(3) . . ?
C21 Pt1 I1 92.0(2) . . ?
C22 Pt1 I1 92.1(2) . . ?
C20 Pt1 I1 176.3(2) . . ?
Sb2 Pt1 I1 87.65(2) . . ?
Sb1 Pt1 I1 86.14(2) . . ?
C1 Sb1 C2 91.2(3) . . ?
C1 Sb1 C3 94.6(3) . . ?
C2 Sb1 C3 111.9(3) . . ?
C1 Sb1 Pt1 104.62(18) . . ?
C2 Sb1 Pt1 125.1(2) . . ?
C3 Sb1 Pt1 118.4(2) . . ?
C18 Sb2 C17 100.5(3) . . ?
C18 Sb2 C19 98.5(3) . . ?
C17 Sb2 C19 103.5(3) . . ?
C18 Sb2 Pt1 112.6(2) . . ?
C17 Sb2 Pt1 121.3(2) . . ?
C19 Sb2 Pt1 117.0(2) . . ?
C9 N1 C11 110.7(6) . . ?
C9 N1 C10 109.1(6) . . ?
C11 N1 C10 109.9(7) . . ?
Sb1 C1 H1A 109.5 . . ?
Sb1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Sb1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Sb1 C2 H2A 109.5 . . ?
Sb1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Sb1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 119.5(7) . . ?
C4 C3 Sb1 118.6(6) . . ?
C8 C3 Sb1 121.8(6) . . ?
C3 C4 C5 121.4(8) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 119.8(9) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.0(8) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.5(8) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C3 C8 C7 118.8(8) . . ?
C3 C8 C9 121.4(7) . . ?
C7 C8 C9 119.9(7) . . ?
N1 C9 C8 112.5(6) . . ?
N1 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
N1 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 114.1(6) . . ?
N1 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
N1 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C13 C12 C17 117.7(7) . . ?
C13 C12 C11 120.2(7) . . ?
C17 C12 C11 122.0(7) . . ?
C14 C13 C12 122.0(8) . . ?
C14 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C15 C14 C13 119.4(8) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 120.2(8) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C17 120.6(7) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C12 120.1(7) . . ?
C16 C17 Sb2 117.5(6) . . ?
C12 C17 Sb2 122.4(6) . . ?
Sb2 C18 H18A 109.5 . . ?
Sb2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Sb2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Sb2 C19 H19A 109.5 . . ?
Sb2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Sb2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Pt1 C20 H20A 109.5 . . ?
Pt1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Pt1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Pt1 C21 H21A 109.5 . . ?
Pt1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Pt1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Pt1 C22 H22A 109.5 . . ?
Pt1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Pt1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.334
_refine_diff_density_min         -1.491
_refine_diff_density_rms         0.242

#===END OF CIF ==============================================================
#
# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set.
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./
#
#===END OF FILE =============================================================