#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:53:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179133 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/95/4309549.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_4309549
loop_
_publ_author_name
'Richard D. Adams'
'Burjor Captain'
'Rolfe H. Herber'
'Mikael Johansson'
'Israel Nowik'
'Jack L. Smith'
'Mark D. Smith'
_publ_section_title
;
Addition of Palladium and Platinum Tri-tert-Butylphosphine Groups to
Re-Sn and Re-Ge Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6346
_journal_page_last               6358
_journal_paper_doi               10.1021/ic051077x
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C32 H20 O8 Re2 Sn2'
_chemical_formula_sum            'C32 H20 O8 Re2 Sn2'
_chemical_formula_weight         1142.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.2830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7904(6)
_cell_length_b                   10.8809(5)
_cell_length_c                   24.0014(12)
_cell_measurement_reflns_used    6062
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.48
_cell_volume                     3263.8(3)
_computing_cell_refinement       'SAINT+  V6.2 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT+  V6.2'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12208
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    8.954
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.1875P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0551
_reflns_number_gt                3597
_reflns_number_total             4028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051077xsi20050630_093546.cif
_cod_data_source_block           re2sn2m296
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4309549
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'
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
Re1 Re 0.136099(9) 0.797319(10) 0.006561(5) 0.03155(5) Uani 1 1 d . . .
Sn1 Sn 0.318318(17) 0.800212(18) 0.091934(9) 0.03337(6) Uani 1 1 d . . .
O11 O 0.0490(2) 0.9247(3) 0.10161(12) 0.0599(7) Uani 1 1 d . . .
O12 O 0.0946(2) 0.5327(3) 0.04872(13) 0.0662(8) Uani 1 1 d . . .
O13 O -0.0875(2) 0.7930(3) -0.07299(16) 0.0751(10) Uani 1 1 d . . .
O14 O 0.1876(2) 1.0612(3) -0.03051(13) 0.0624(7) Uani 1 1 d . . .
C11 C 0.0839(3) 0.8738(3) 0.06799(14) 0.0397(7) Uani 1 1 d . . .
C12 C 0.1097(2) 0.6280(3) 0.03321(16) 0.0431(8) Uani 1 1 d . . .
C13 C -0.0031(3) 0.7939(3) -0.04472(19) 0.0498(9) Uani 1 1 d . . .
C14 C 0.1703(2) 0.9635(3) -0.01783(15) 0.0413(7) Uani 1 1 d . . .
C21 C 0.3902(2) 0.9703(3) 0.12492(14) 0.0378(7) Uani 1 1 d . . .
C22 C 0.3458(3) 1.0833(3) 0.10996(19) 0.0568(10) Uani 1 1 d . . .
H22 H 0.2805 1.0885 0.0841 0.068 Uiso 1 1 calc R . .
C23 C 0.3967(5) 1.1903(4) 0.1328(2) 0.0738(14) Uani 1 1 d . . .
H23 H 0.3655 1.2663 0.1222 0.089 Uiso 1 1 calc R . .
C24 C 0.4920(5) 1.1840(4) 0.1706(2) 0.0733(14) Uani 1 1 d . . .
H24 H 0.5256 1.2556 0.1862 0.088 Uiso 1 1 calc R . .
C25 C 0.5381(3) 1.0732(4) 0.1854(2) 0.0705(13) Uani 1 1 d . . .
H25 H 0.6041 1.0690 0.2107 0.085 Uiso 1 1 calc R . .
C26 C 0.4875(3) 0.9664(4) 0.16310(17) 0.0556(9) Uani 1 1 d . . .
H26 H 0.5194 0.8909 0.1740 0.067 Uiso 1 1 calc R . .
C27 C 0.3281(3) 0.6924(3) 0.16750(16) 0.0413(7) Uani 1 1 d . . .
C28 C 0.3426(4) 0.5672(4) 0.1703(2) 0.0719(12) Uani 1 1 d . . .
H28 H 0.3491 0.5240 0.1378 0.086 Uiso 1 1 calc R . .
C29 C 0.3477(5) 0.5044(5) 0.2212(2) 0.0943(17) Uani 1 1 d . . .
H29 H 0.3578 0.4197 0.2225 0.113 Uiso 1 1 calc R . .
C30 C 0.3382(4) 0.5656(5) 0.2690(2) 0.0824(15) Uani 1 1 d . . .
H30 H 0.3417 0.5228 0.3029 0.099 Uiso 1 1 calc R . .
C31 C 0.3237(4) 0.6882(5) 0.2676(2) 0.0793(16) Uani 1 1 d . . .
H31 H 0.3165 0.7301 0.3003 0.095 Uiso 1 1 calc R . .
C32 C 0.3195(4) 0.7520(4) 0.21684(18) 0.0607(10) Uani 1 1 d . . .
H32 H 0.3106 0.8368 0.2163 0.073 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'
O O 0.0106 0.0060 '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'
Re Re -1.0185 7.2310 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 Re1 C13 94.21(15) . . ?
C11 Re1 C14 88.06(14) . . ?
C13 Re1 C14 93.48(14) . . ?
C11 Re1 C12 92.50(14) . . ?
C13 Re1 C12 89.48(14) . . ?
C14 Re1 C12 176.94(13) . . ?
C11 Re1 Sn1 78.60(9) . . ?
C13 Re1 Sn1 171.80(13) . . ?
C14 Re1 Sn1 90.24(9) . . ?
C12 Re1 Sn1 86.93(9) . . ?
C11 Re1 Sn1 171.21(10) . 7_565 ?
C13 Re1 Sn1 77.39(12) . 7_565 ?
C14 Re1 Sn1 89.86(10) . 7_565 ?
C12 Re1 Sn1 90.03(10) . 7_565 ?
Sn1 Re1 Sn1 109.955(7) . 7_565 ?
C11 Re1 Re1 133.65(10) . 7_565 ?
C13 Re1 Re1 132.12(12) . 7_565 ?
C14 Re1 Re1 90.09(9) . 7_565 ?
C12 Re1 Re1 87.35(9) . 7_565 ?
Sn1 Re1 Re1 55.088(6) . 7_565 ?
Sn1 Re1 Re1 54.866(6) 7_565 7_565 ?
C27 Sn1 C21 102.54(12) . . ?
C27 Sn1 Re1 120.75(9) . . ?
C21 Sn1 Re1 120.87(8) . . ?
C27 Sn1 Re1 121.94(9) . 7_565 ?
C21 Sn1 Re1 119.73(9) . 7_565 ?
Re1 Sn1 Re1 70.045(7) . 7_565 ?
O11 C11 Re1 175.2(3) . . ?
O12 C12 Re1 179.4(3) . . ?
O13 C13 Re1 176.9(4) . . ?
O14 C14 Re1 177.2(3) . . ?
C22 C21 C26 117.7(3) . . ?
C22 C21 Sn1 123.9(2) . . ?
C26 C21 Sn1 118.4(3) . . ?
C21 C22 C23 121.1(4) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 120.1(4) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 119.9(4) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 120.2(4) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 121.0(4) . . ?
C21 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C28 C27 C32 117.4(4) . . ?
C28 C27 Sn1 124.6(3) . . ?
C32 C27 Sn1 118.0(3) . . ?
C27 C28 C29 120.7(5) . . ?
C27 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
C30 C29 C28 120.5(5) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C31 C30 C29 120.2(5) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C32 119.6(5) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C27 C32 C31 121.5(4) . . ?
C27 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
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
Re1 C11 1.931(3) . ?
Re1 C13 1.937(4) . ?
Re1 C14 1.978(4) . ?
Re1 C12 2.003(4) . ?
Re1 Sn1 2.7567(3) . ?
Re1 Sn1 2.7643(3) 7_565 ?
Re1 Re1 3.1685(3) 7_565 ?
Sn1 C27 2.141(3) . ?
Sn1 C21 2.141(3) . ?
Sn1 Re1 2.7643(3) 7_565 ?
O11 C11 1.145(4) . ?
O12 C12 1.132(4) . ?
O13 C13 1.147(4) . ?
O14 C14 1.140(4) . ?
C21 C22 1.371(5) . ?
C21 C26 1.380(5) . ?
C22 C23 1.388(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.356(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.357(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.381(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.374(5) . ?
C27 C32 1.375(5) . ?
C28 C29 1.389(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.353(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.347(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.393(6) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
