#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:53:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179133 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/95/4309550.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_4309550
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 Ge2 O8 Re2'
_chemical_formula_sum            'C32 H20 Ge2 O8 Re2'
_chemical_formula_weight         1050.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 117.3840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.0667(11)
_cell_length_b                   10.6056(8)
_cell_length_c                   12.0970(10)
_cell_measurement_reflns_used    2835
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.52
_cell_volume                     1602.5(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6632
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    9.435
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0254
_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)+(0.0327P)²+0.8388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                1410
_reflns_number_total             1505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051077xsi20050630_093746.cif
_cod_data_source_block           Re2Ge2
_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               4309550
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.0000 0.14384(3) 0.5000 0.04400(12) Uani 1 2 d S . .
Ge1 Ge 0.14097(6) 0.0000 0.66937(7) 0.0478(2) Uani 1 2 d S . .
O11 O 0.1152(4) 0.1516(4) 0.3325(5) 0.0833(14) Uani 1 1 d . . .
O12 O 0.1654(4) 0.3420(4) 0.6625(5) 0.0791(13) Uani 1 1 d . . .
C11 C 0.0740(4) 0.1453(5) 0.3927(5) 0.0556(13) Uani 1 1 d . . .
C12 C 0.1048(4) 0.2677(5) 0.6056(5) 0.0533(13) Uani 1 1 d . . .
C21 C 0.1445(6) 0.0000 0.8342(6) 0.0531(18) Uani 1 2 d S . .
C22 C 0.1449(6) 0.1100(6) 0.8931(6) 0.082(2) Uani 1 1 d . . .
H22 H 0.1422 0.1865 0.8543 0.098 Uiso 1 1 d R . .
C23 C 0.1488(7) 0.1091(7) 1.0107(7) 0.093(2) Uani 1 1 d . . .
H23 H 0.1494 0.1849 1.0496 0.112 Uiso 1 1 d R . .
C24 C 0.1511(8) 0.0000 1.0667(9) 0.081(3) Uani 1 2 d S . .
H24 H 0.1551 0.0000 1.1457 0.098 Uiso 1 2 d SR . .
C25 C 0.2909(6) 0.0000 0.7031(7) 0.058(2) Uani 1 2 d S . .
C26 C 0.3238(6) 0.0000 0.6126(8) 0.060(2) Uani 1 2 d S . .
H26 H 0.2722 0.0000 0.5296 0.072 Uiso 1 2 d SR . .
C27 C 0.4301(7) 0.0000 0.6401(9) 0.066(2) Uani 1 2 d S . .
H27 H 0.4498 0.0000 0.5723 0.079 Uiso 1 2 d SR . .
C28 C 0.5056(8) 0.028(2) 0.7585(11) 0.074(8) Uani 0.50 1 d P . .
H28 H 0.5802 0.0263 0.7924 0.089 Uiso 0.50 1 d PR . .
C29 C 0.4768(8) 0.0542(13) 0.8485(11) 0.083(5) Uani 0.50 1 d P . .
H29 H 0.5210 0.0831 0.9259 0.100 Uiso 0.50 1 d PR . .
C30 C 0.3689(8) 0.0501(11) 0.8214(10) 0.067(4) Uani 0.50 1 d P . .
H30 H 0.3311 0.0539 0.8734 0.081 Uiso 0.50 1 d PR . .
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'
Ge Ge 0.1547 1.8001 '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
C12 Re1 C12 95.2(3) . 2_556 ?
C12 Re1 C11 91.8(2) . 2_556 ?
C12 Re1 C11 87.6(2) 2_556 2_556 ?
C12 Re1 C11 87.6(2) . . ?
C12 Re1 C11 91.8(2) 2_556 . ?
C11 Re1 C11 179.1(3) 2_556 . ?
C12 Re1 Ge1 171.01(16) . 5_556 ?
C12 Re1 Ge1 78.79(16) 2_556 5_556 ?
C11 Re1 Ge1 94.59(15) 2_556 5_556 ?
C11 Re1 Ge1 85.94(17) . 5_556 ?
C12 Re1 Ge1 78.79(16) . . ?
C12 Re1 Ge1 171.01(16) 2_556 . ?
C11 Re1 Ge1 85.94(17) 2_556 . ?
C11 Re1 Ge1 94.59(15) . . ?
Ge1 Re1 Ge1 107.90(2) 5_556 . ?
C12 Re1 Re1 132.38(16) . 5_556 ?
C12 Re1 Re1 132.38(16) 2_556 5_556 ?
C11 Re1 Re1 90.45(15) 2_556 5_556 ?
C11 Re1 Re1 90.45(15) . 5_556 ?
Ge1 Re1 Re1 53.951(11) 5_556 5_556 ?
Ge1 Re1 Re1 53.951(11) . 5_556 ?
C25 Ge1 C21 105.4(3) . . ?
C25 Ge1 Re1 121.65(16) . 5_556 ?
C21 Ge1 Re1 116.98(15) . 5_556 ?
C25 Ge1 Re1 121.65(16) . . ?
C21 Ge1 Re1 116.98(15) . . ?
Re1 Ge1 Re1 72.10(2) 5_556 . ?
O11 C11 Re1 177.1(5) . . ?
O12 C12 Re1 177.1(5) . . ?
C22 C21 C22 117.4(8) . 6 ?
C22 C21 Ge1 121.3(4) . . ?
C21 C22 C23 120.9(7) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 120.2(7) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C23 120.3(9) 6 . ?
C23 C24 H24 119.9 . . ?
C26 C25 C30 114.1(7) . . ?
C26 C25 Ge1 124.2(6) . . ?
C30 C25 Ge1 117.5(6) . . ?
C25 C26 C27 122.4(8) . . ?
C25 C26 H26 118.7 . . ?
C27 C26 H26 118.9 . . ?
C28 C27 C26 119.2(8) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.5 . . ?
C29 C28 C27 120.8(10) . . ?
C29 C28 H28 110.1 . . ?
C27 C28 H28 129.0 . . ?
C28 C29 C30 119.9(11) . . ?
C28 C29 H29 125.7 . . ?
C30 C29 H29 114.0 . . ?
C29 C30 C25 119.5(10) . . ?
C29 C30 H30 133.5 . . ?
C25 C30 H30 104.9 . . ?
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 C12 1.949(6) . ?
Re1 C12 1.949(6) 2_556 ?
Re1 C11 2.003(6) 2_556 ?
Re1 C11 2.003(6) . ?
Re1 Ge1 2.5923(6) 5_556 ?
Re1 Ge1 2.5923(6) . ?
Re1 Re1 3.0510(6) 5_556 ?
Ge1 C25 1.955(7) . ?
Ge1 C21 1.972(7) . ?
Ge1 Re1 2.5923(6) 5_556 ?
O11 C11 1.122(7) . ?
O12 C12 1.132(6) . ?
C21 C22 1.365(7) . ?
C21 C22 1.365(7) 6 ?
C22 C23 1.397(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.334(8) . ?
C23 H23 0.9300 . ?
C24 C23 1.334(8) 6 ?
C24 H24 0.9300 . ?
C25 C26 1.372(10) . ?
C25 C30 1.445(12) . ?
C25 C30 1.445(12) 6 ?
C26 C27 1.374(11) . ?
C26 H26 0.9300 . ?
C27 C28 1.367(14) . ?
C27 C28 1.367(14) 6 ?
C27 H27 0.9800 . ?
C28 C29 1.353(16) . ?
C28 H28 0.9353 . ?
C29 C30 1.398(14) . ?
C29 H29 0.9066 . ?
C30 H30 0.9947 . ?
