#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:59:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179224 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/46/4314602.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_4314602
loop_
_publ_author_name
'Fei Cheng'
'Andrew L. Hector'
'William Levason'
'Gillian Reid'
'Michael Webster'
'Wenjian Zhang'
_publ_contact_author_address
;   School of Chemistry
    University of Southampton
    Southampton SO17 1BJ, UK
;
_publ_contact_author_email       gr@soton.ac.uk
_publ_contact_author_fax         '023 8059 3781'
_publ_contact_author_name        'Professor Gillian Reid'
_publ_contact_author_phone       '023 8059 3609'
_publ_section_title
;
 Diphosphine and Diarsine Complexes of Germanium(II) Halides-Preparation,
 Spectroscopic, and Structural Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              752
_journal_page_last               760
_journal_paper_doi               10.1021/ic902068z
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C30 H24 Ge I2 P2'
_chemical_formula_sum            'C30 H24 Ge I2 P2'
_chemical_formula_weight         772.82
_chemical_name_systematic
; 
 diiodo-1,2-bis(diphenylphosphino)benzene-germanium(II) 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Zhang, W.'
_audit_creation_date             2009-09-18
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 97.270(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0465(18)
_cell_length_b                   14.192(3)
_cell_length_c                   18.503(3)
_cell_measurement_reflns_used    6364
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2877.4(9)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30988
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         3.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.339
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0344P)²+46.7960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                5059
_reflns_number_total             6526
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic902068z_si_001_09.cif
_cod_data_source_block           09wz930
_cod_original_cell_volume        2877.5(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4314602
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'
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
Ge1 Ge -0.11718(8) 0.63746(6) 0.10195(5) 0.0248(2) Uani 1 1 d . . .
I1 I 0.00239(5) 0.66740(4) 0.23481(3) 0.02952(16) Uani 1 1 d . . .
I2 I -0.34582(5) 0.69362(4) 0.13121(3) 0.03217(17) Uani 1 1 d . . .
P1 P -0.05889(19) 0.79918(14) 0.06352(11) 0.0221(4) Uani 1 1 d . . .
P2 P 0.13586(19) 0.63819(14) 0.05008(11) 0.0225(4) Uani 1 1 d . . .
C1 C -0.0916(7) 0.7990(5) -0.0347(4) 0.0223(16) Uani 1 1 d . . .
C2 C -0.0137(8) 0.8385(6) -0.0796(5) 0.0279(18) Uani 1 1 d . . .
H2 H 0.0591 0.8692 -0.0591 0.034 Uiso 1 1 calc R . .
C3 C -0.0430(8) 0.8330(6) -0.1550(5) 0.0295(18) Uani 1 1 d . . .
H3 H 0.0094 0.8606 -0.1861 0.035 Uiso 1 1 calc R . .
C4 C -0.1476(10) 0.7875(7) -0.1845(5) 0.039(2) Uani 1 1 d . . .
H4 H -0.1665 0.7839 -0.2360 0.047 Uiso 1 1 calc R . .
C5 C -0.2245(9) 0.7475(7) -0.1417(5) 0.035(2) Uani 1 1 d . . .
H5 H -0.2959 0.7158 -0.1631 0.042 Uiso 1 1 calc R . .
C6 C -0.1983(8) 0.7530(6) -0.0658(4) 0.0272(18) Uani 1 1 d . . .
H6 H -0.2523 0.7258 -0.0355 0.033 Uiso 1 1 calc R . .
C7 C -0.1431(8) 0.8975(6) 0.0947(5) 0.0288(18) Uani 1 1 d . . .
C8 C -0.1324(9) 0.9175(6) 0.1681(5) 0.034(2) Uani 1 1 d . . .
H8 H -0.0811 0.8799 0.2017 0.040 Uiso 1 1 calc R . .
C9 C -0.1970(9) 0.9935(7) 0.1934(6) 0.041(2) Uani 1 1 d . . .
H9 H -0.1885 1.0081 0.2439 0.049 Uiso 1 1 calc R . .
C10 C -0.2730(11) 1.0468(7) 0.1442(6) 0.049(3) Uani 1 1 d . . .
H10 H -0.3163 1.0986 0.1609 0.059 Uiso 1 1 calc R . .
C11 C -0.2864(11) 1.0250(7) 0.0703(7) 0.051(3) Uani 1 1 d . . .
H11 H -0.3402 1.0612 0.0371 0.061 Uiso 1 1 calc R . .
C12 C -0.2217(10) 0.9505(7) 0.0445(6) 0.042(2) Uani 1 1 d . . .
H12 H -0.2305 0.9358 -0.0060 0.050 Uiso 1 1 calc R . .
C13 C 0.1032(7) 0.8265(6) 0.0865(4) 0.0235(16) Uani 1 1 d . . .
C14 C 0.1395(8) 0.9162(6) 0.1105(5) 0.0265(17) Uani 1 1 d . . .
H14 H 0.0803 0.9642 0.1133 0.032 Uiso 1 1 calc R . .
C15 C 0.2631(9) 0.9357(6) 0.1305(5) 0.032(2) Uani 1 1 d . . .
H15 H 0.2878 0.9968 0.1474 0.039 Uiso 1 1 calc R . .
C16 C 0.3498(9) 0.8664(6) 0.1258(5) 0.0321(19) Uani 1 1 d . . .
H16 H 0.4337 0.8797 0.1400 0.039 Uiso 1 1 calc R . .
C17 C 0.3136(8) 0.7760(6) 0.1000(5) 0.0290(18) Uani 1 1 d . . .
H17 H 0.3735 0.7290 0.0960 0.035 Uiso 1 1 calc R . .
C18 C 0.1902(8) 0.7549(6) 0.0801(4) 0.0260(17) Uani 1 1 d . . .
C19 C 0.2630(7) 0.5594(5) 0.0834(5) 0.0241(16) Uani 1 1 d . . .
C20 C 0.3253(8) 0.5070(6) 0.0376(5) 0.0264(17) Uani 1 1 d . . .
H20 H 0.3049 0.5121 -0.0137 0.032 Uiso 1 1 calc R . .
C21 C 0.4196(8) 0.4457(6) 0.0670(5) 0.0271(17) Uani 1 1 d . . .
H21 H 0.4632 0.4099 0.0354 0.032 Uiso 1 1 calc R . .
C22 C 0.4479(8) 0.4379(6) 0.1402(5) 0.0309(19) Uani 1 1 d . . .
H22 H 0.5117 0.3968 0.1597 0.037 Uiso 1 1 calc R . .
C23 C 0.3844(9) 0.4896(7) 0.1871(5) 0.035(2) Uani 1 1 d . . .
H23 H 0.4059 0.4846 0.2383 0.042 Uiso 1 1 calc R . .
C24 C 0.2900(8) 0.5482(6) 0.1591(4) 0.0269(17) Uani 1 1 d . . .
H24 H 0.2436 0.5809 0.1910 0.032 Uiso 1 1 calc R . .
C25 C 0.1379(8) 0.6405(6) -0.0482(5) 0.0284(18) Uani 1 1 d . . .
C26 C 0.0407(9) 0.5976(6) -0.0911(5) 0.0309(19) Uani 1 1 d . . .
H26 H -0.0229 0.5692 -0.0687 0.037 Uiso 1 1 calc R . .
C27 C 0.0362(9) 0.5963(6) -0.1666(5) 0.034(2) Uani 1 1 d . . .
H27 H -0.0302 0.5667 -0.1956 0.041 Uiso 1 1 calc R . .
C28 C 0.1299(11) 0.6386(7) -0.1998(5) 0.044(3) Uani 1 1 d . . .
H28 H 0.1270 0.6378 -0.2514 0.052 Uiso 1 1 calc R . .
C29 C 0.2262(10) 0.6814(7) -0.1576(5) 0.038(2) Uani 1 1 d . . .
H29 H 0.2896 0.7102 -0.1800 0.046 Uiso 1 1 calc R . .
C30 C 0.2306(8) 0.6826(6) -0.0816(5) 0.0286(18) Uani 1 1 d . . .
H30 H 0.2970 0.7121 -0.0527 0.034 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'
P P 0.1023 0.0942 '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'
I I -0.4742 1.8119 '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
P1 Ge1 I1 90.03(6) . . ?
P1 Ge1 I2 93.74(6) . . ?
I1 Ge1 I2 97.55(3) . . ?
P1 Ge1 P2 68.40(6) . . ?
I1 Ge1 P2 85.61(5) . . ?
I2 Ge1 P2 161.93(5) . . ?
C1 P1 C7 106.0(4) . . ?
C1 P1 C13 107.4(4) . . ?
C7 P1 C13 106.9(4) . . ?
C1 P1 Ge1 104.9(3) . . ?
C7 P1 Ge1 117.0(3) . . ?
C13 P1 Ge1 114.0(3) . . ?
C25 P2 C18 104.0(4) . . ?
C25 P2 C19 103.9(4) . . ?
C18 P2 C19 104.0(4) . . ?
C25 P2 Ge1 116.1(3) . . ?
C18 P2 Ge1 100.7(3) . . ?
C19 P2 Ge1 125.5(3) . . ?
C2 C1 C6 119.6(8) . . ?
C2 C1 P1 122.7(6) . . ?
C6 C1 P1 117.6(6) . . ?
C1 C2 C3 119.5(8) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 120.1(9) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 121.4(9) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 119.8(9) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 119.6(8) . . ?
C5 C6 H6 120.2 . . ?
C1 C6 H6 120.2 . . ?
C8 C7 C12 120.6(8) . . ?
C8 C7 P1 119.3(7) . . ?
C12 C7 P1 120.0(7) . . ?
C7 C8 C9 120.2(9) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 119.4(9) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 120.4(9) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C12 120.7(10) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 118.6(10) . . ?
C11 C12 H12 120.7 . . ?
C7 C12 H12 120.7 . . ?
C14 C13 C18 120.8(8) . . ?
C14 C13 P1 120.2(6) . . ?
C18 C13 P1 119.0(6) . . ?
C13 C14 C15 119.9(8) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 120.3(8) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 119.9(8) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C18 C17 C16 120.7(8) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C13 118.3(8) . . ?
C17 C18 P2 123.1(6) . . ?
C13 C18 P2 118.5(6) . . ?
C20 C19 C24 119.6(8) . . ?
C20 C19 P2 122.8(6) . . ?
C24 C19 P2 117.4(6) . . ?
C19 C20 C21 119.9(8) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 120.1(8) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.6(8) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C23 C22 120.0(8) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C19 119.8(8) . . ?
C23 C24 H24 120.1 . . ?
C19 C24 H24 120.1 . . ?
C26 C25 C30 119.4(8) . . ?
C26 C25 P2 117.1(7) . . ?
C30 C25 P2 123.5(7) . . ?
C27 C26 C25 120.4(9) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 119.9(9) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 119.9(9) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.0(9) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C25 C30 C29 120.4(9) . . ?
C25 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
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
Ge1 P1 2.511(2) . ?
Ge1 I1 2.6733(11) . ?
Ge1 I2 2.7663(11) . ?
Ge1 P2 3.068(2) . ?
P1 C1 1.807(8) . ?
P1 C7 1.811(8) . ?
P1 C13 1.829(8) . ?
P2 C25 1.823(9) . ?
P2 C18 1.825(9) . ?
P2 C19 1.839(8) . ?
C1 C2 1.388(12) . ?
C1 C6 1.406(12) . ?
C2 C3 1.395(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.375(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.358(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(13) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.377(13) . ?
C7 C12 1.407(13) . ?
C8 C9 1.406(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(16) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(13) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.391(11) . ?
C13 C18 1.413(12) . ?
C14 C15 1.396(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.409(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.398(12) . ?
C17 H17 0.9500 . ?
C19 C20 1.375(12) . ?
C19 C24 1.404(12) . ?
C20 C21 1.412(11) . ?
C20 H20 0.9500 . ?
C21 C22 1.356(12) . ?
C21 H21 0.9500 . ?
C22 C23 1.391(13) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(12) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.392(13) . ?
C25 C30 1.395(13) . ?
C26 C27 1.391(13) . ?
C26 H26 0.9500 . ?
C27 C28 1.404(15) . ?
C27 H27 0.9500 . ?
C28 C29 1.379(15) . ?
C28 H28 0.9500 . ?
C29 C30 1.400(13) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
