Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002


data_oct901

_database_code_CSD	174129


_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Francis, Matthew D.'
'Hitchcock, Peter B.'

_publ_contact_author_name     	'Matthew D Francis'  
_publ_contact_author_address 
;
School of Chemistry, Physics and Environmental Sciences
Sussex University
Brighton
BN1 9QJ
UNITED KINGDOM
;

_publ_contact_author_email       'M.D.FRANCIS@SUSSEX.AC.UK'

_publ_section_title		
;
Synthesis, crystal and molecular structure of [Sn(n4-P2C2But2)]: the
first non transitional metal 1,3-diphosphacyclobutadienyl compound
;

_audit_creation_date            2001-10-11T15:35:43-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.1
_audit_conform_dict_location    ftp://ftp.iucr.org/cifdics/cif_core.dic
_publ_requested_category        FM

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic
;
?
;
_chemical_name_common                   '[Sn(P2(CtBu)2}]'
_chemical_formula_moiety                'C10 H18 P2 Sn1'
_chemical_formula_sum                   'C10 H18 P2 Sn'
_chemical_formula_weight                318.87
_chemical_compound_source               'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          C2/c
_symmetry_Int_Tables_number             15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'

_cell_length_a                          19.812(2)
_cell_length_b                          6.0863(8)
_cell_length_c                          10.6752(13)
_cell_angle_alpha                       90
_cell_angle_beta                        96.024(7)
_cell_angle_gamma                       90
_cell_volume                            1280.1(3)
_cell_formula_units_Z                   4
_cell_measurement_temperature           173(2)
_cell_measurement_reflns_used           4890
_cell_measurement_theta_min             3.705
_cell_measurement_theta_max             25.028
_cell_measurement_wavelength            0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description              plate
_exptl_crystal_colour                   yellow
_exptl_crystal_size_max                 0.3
_exptl_crystal_size_mid                 0.3
_exptl_crystal_size_min                 0.05
_exptl_crystal_density_diffrn           1.655
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    632
_exptl_special_details
;
?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu           2.205
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min         0.635
_exptl_absorpt_correction_T_max         0.831

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature             173(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_measurement_device              KappaCCD
_diffrn_measurement_method              CCD
_diffrn_reflns_number                   2518
_diffrn_reflns_av_R_equivalents         0.0571
_diffrn_reflns_av_unetI/netI            0.0568
_diffrn_reflns_limit_h_min              -21
_diffrn_reflns_limit_h_max              23
_diffrn_reflns_limit_k_min              -7
_diffrn_reflns_limit_k_max              6
_diffrn_reflns_limit_l_min              -10
_diffrn_reflns_limit_l_max              12
_diffrn_reflns_theta_min                3.94
_diffrn_reflns_theta_max                24.99
_diffrn_reflns_theta_full               24.99
_diffrn_measured_fraction_theta_full	0.981
_diffrn_measured_fraction_theta_max	0.981
_reflns_number_total                    1115
_reflns_number_gt                       998
_reflns_threshold_expression            >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_cell_refinement
'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] 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           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                1115
_refine_ls_number_parameters            60
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0389
_refine_ls_R_factor_gt                  0.0336
_refine_ls_wR_factor_ref                0.0859
_refine_ls_wR_factor_gt                 0.0831
_refine_ls_goodness_of_fit_ref          1.073
_refine_ls_restrained_S_all             1.073
_refine_ls_shift/su_max                 0
_refine_ls_shift/su_mean                0
_refine_diff_density_max                1.206
_refine_diff_density_min                -0.837
_refine_diff_density_rms                0.114

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Sn Sn 0 0.06573(5) 0.25 0.0368(2) Uani 1 2 d S . .
P P -0.02037(4) -0.30129(15) 0.36694(7) 0.0284(3) Uani 1 1 d . . .
C1 C 0.05721(17) -0.2836(5) 0.2942(3) 0.0243(7) Uani 1 1 d . . .
C2 C 0.13027(17) -0.2992(5) 0.3495(3) 0.0256(7) Uani 1 1 d . . .
C3 C 0.1498(2) -0.5432(6) 0.3655(4) 0.0332(9) Uani 1 1 d . . .
H3A H 0.1972 -0.5551 0.4014 0.05 Uiso 1 1 calc R . .
H3B H 0.1441 -0.6161 0.2832 0.05 Uiso 1 1 calc R . .
H3C H 0.1204 -0.6139 0.422 0.05 Uiso 1 1 calc R . .
C4 C 0.13967(19) -0.1902(6) 0.4798(3) 0.0366(8) Uani 1 1 d . . .
H4A H 0.1873 -0.2024 0.5148 0.055 Uiso 1 1 calc R . .
H4B H 0.1107 -0.2639 0.5359 0.055 Uiso 1 1 calc R . .
H4C H 0.127 -0.0348 0.4719 0.055 Uiso 1 1 calc R . .
C5 C 0.17754(19) -0.1910(6) 0.2623(4) 0.0367(8) Uani 1 1 d . . .
H5A H 0.2247 -0.2039 0.2998 0.055 Uiso 1 1 calc R . .
H5B H 0.1657 -0.0354 0.2512 0.055 Uiso 1 1 calc R . .
H5C H 0.1724 -0.2646 0.1802 0.055 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
Sn 0.0333(3) 0.0220(2) 0.0535(3) 0 -0.00288(18) 0
P 0.0274(5) 0.0368(5) 0.0213(4) 0.0035(4) 0.0043(4) 0.0006(4)
C1 0.0290(18) 0.0213(16) 0.0236(15) 0.0020(13) 0.0069(13) 0.0021(13)
C2 0.0224(16) 0.0266(17) 0.0277(16) 0.0008(14) 0.0022(12) 0.0001(13)
C3 0.028(2) 0.030(2) 0.040(2) 0.0024(15) 0.0008(16) 0.0038(15)
C4 0.035(2) 0.042(2) 0.0305(18) -0.0059(17) -0.0052(15) 0.0041(17)
C5 0.0289(19) 0.044(2) 0.0369(18) 0.0064(17) 0.0034(15) -0.0049(16)


#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Sn C1 2.432(3) 6_556 ?
Sn C1 2.432(3) . ?
Sn P 2.6109(10) 6_556 ?
Sn P 2.6109(10) . ?
P C1 1.796(3) . ?
P C1 1.800(3) 6_556 ?
C1 C2 1.508(5) . ?
C1 P 1.800(3) 6_556 ?
C2 C4 1.535(5) . ?
C2 C5 1.536(5) . ?
C2 C3 1.540(5) . ?

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
C1 Sn C1 58.11(16) 6_556 . ?
C1 Sn P 41.55(7) 6_556 6_556 ?
C1 Sn P 41.64(7) . 6_556 ?
C1 Sn P 41.64(7) 6_556 . ?
C1 Sn P 41.55(7) . . ?
P Sn P 62.36(4) 6_556 . ?
C1 P C1 82.11(17) . 6_556 ?
C1 P Sn 63.88(10) . . ?
C1 P Sn 63.85(10) 6_556 . ?
C2 C1 P 131.1(2) . . ?
C2 C1 P 130.3(2) . 6_556 ?
P C1 P 97.47(17) . 6_556 ?
C2 C1 Sn 122.7(2) . . ?
P C1 Sn 74.57(11) . . ?
P C1 Sn 74.51(11) 6_556 . ?
C1 C2 C4 110.4(3) . . ?
C1 C2 C5 110.9(3) . . ?
C4 C2 C5 109.9(3) . . ?
C1 C2 C3 108.9(3) . . ?
C4 C2 C3 108.1(3) . . ?
C5 C2 C3 108.6(3) . . ?