#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:46:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179077 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/39/4303991.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_4303991
loop_
_publ_author_name
'Cameron Jones'
'Christian Schulten'
'Andreas Stasch'
_publ_section_title
;
Unusual Reactivity of Methylphosphaalkyne (P\\tbCMe) toward Digermenes and
Distannenes: Stepwise Formations of Bridged
2,3,5,6-Tetraphospha-1,4-dimethylidenecyclohexanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1273
_journal_page_last               1278
_journal_paper_doi               10.1021/ic700926u
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C23 H44 Ge O5 P2 Si4 W'
_chemical_formula_weight         831.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.46(3)
_cell_angle_beta                 100.06(3)
_cell_angle_gamma                100.66(3)
_cell_formula_units_Z            2
_cell_length_a                   9.836(2)
_cell_length_b                   11.780(2)
_cell_length_c                   16.021(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1758.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15783
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    4.377
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.572
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         8421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0101P)²+1.9207P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0513
_reflns_number_gt                7942
_reflns_number_total             8421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700926u-file001_4.cif
_cod_data_source_block           compound14
_cod_original_cell_volume        1758.9(6)
_cod_database_code               4303991
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
W1 W 0.962396(10) 0.313714(8) 0.349270(6) 0.01799(3) Uani 1 1 d . . .
Ge1 Ge 0.68879(2) -0.14978(2) 0.233833(15) 0.01462(5) Uani 1 1 d . . .
P1 P 0.51071(7) -0.04550(6) 0.20621(4) 0.01956(13) Uani 1 1 d . . .
P2 P 0.79891(6) 0.11633(5) 0.30349(4) 0.01654(12) Uani 1 1 d . . .
Si1 Si 0.55602(8) -0.21945(6) 0.39644(4) 0.02170(14) Uani 1 1 d . . .
Si2 Si 0.49601(8) -0.40768(6) 0.21958(5) 0.02230(15) Uani 1 1 d . . .
Si3 Si 0.92490(7) -0.25806(6) 0.14329(4) 0.02052(14) Uani 1 1 d . . .
Si4 Si 0.71812(8) -0.13008(6) 0.03509(4) 0.02101(14) Uani 1 1 d . . .
O1 O 1.2134(2) 0.1986(2) 0.29976(16) 0.0461(6) Uani 1 1 d . . .
O2 O 0.8997(3) 0.3519(2) 0.15478(14) 0.0556(7) Uani 1 1 d . . .
O3 O 1.1689(2) 0.56425(18) 0.41331(14) 0.0403(5) Uani 1 1 d . . .
O4 O 0.7321(3) 0.4569(2) 0.39479(16) 0.0507(6) Uani 1 1 d . . .
O5 O 1.0434(3) 0.2692(2) 0.54000(13) 0.0434(6) Uani 1 1 d . . .
C1 C 0.6132(2) 0.0897(2) 0.25240(15) 0.0181(5) Uani 1 1 d . . .
C2 C 0.5502(3) 0.1977(2) 0.25493(19) 0.0293(6) Uani 1 1 d . . .
H2A H 0.4494 0.1738 0.2272 0.044 Uiso 1 1 calc R . .
H2B H 0.5992 0.2518 0.2240 0.044 Uiso 1 1 calc R . .
H2C H 0.5610 0.2373 0.3152 0.044 Uiso 1 1 calc R . .
C3 C 0.8380(2) -0.0159(2) 0.30446(15) 0.0167(5) Uani 1 1 d . . .
C4 C 0.9770(3) -0.0264(2) 0.35561(16) 0.0215(5) Uani 1 1 d . . .
H4A H 1.0287 0.0514 0.3895 0.032 Uiso 1 1 calc R . .
H4B H 1.0333 -0.0568 0.3159 0.032 Uiso 1 1 calc R . .
H4C H 0.9596 -0.0806 0.3948 0.032 Uiso 1 1 calc R . .
C5 C 0.6221(3) -0.2750(2) 0.29618(15) 0.0184(5) Uani 1 1 d . . .
H5 H 0.7082 -0.3041 0.3181 0.022 Uiso 1 1 calc R . .
C6 C 0.6673(3) -0.0745(3) 0.46140(18) 0.0348(7) Uani 1 1 d . . .
H6A H 0.6529 -0.0118 0.4298 0.052 Uiso 1 1 calc R . .
H6B H 0.7673 -0.0785 0.4711 0.052 Uiso 1 1 calc R . .
H6C H 0.6397 -0.0576 0.5173 0.052 Uiso 1 1 calc R . .
C7 C 0.3710(3) -0.1983(3) 0.36808(19) 0.0300(6) Uani 1 1 d . . .
H7A H 0.3098 -0.2713 0.3318 0.045 Uiso 1 1 calc R . .
H7B H 0.3699 -0.1340 0.3363 0.045 Uiso 1 1 calc R . .
H7C H 0.3364 -0.1786 0.4212 0.045 Uiso 1 1 calc R . .
C8 C 0.5634(3) -0.3254(3) 0.47196(18) 0.0335(7) Uani 1 1 d . . .
H8A H 0.5395 -0.2915 0.5262 0.050 Uiso 1 1 calc R . .
H8B H 0.6590 -0.3401 0.4841 0.050 Uiso 1 1 calc R . .
H8C H 0.4954 -0.3999 0.4450 0.050 Uiso 1 1 calc R . .
C9 C 0.3650(3) -0.3603(3) 0.1405(2) 0.0351(7) Uani 1 1 d . . .
H9A H 0.2956 -0.4299 0.1055 0.053 Uiso 1 1 calc R . .
H9B H 0.4145 -0.3186 0.1026 0.053 Uiso 1 1 calc R . .
H9C H 0.3162 -0.3077 0.1720 0.053 Uiso 1 1 calc R . .
C10 C 0.5902(3) -0.5062(2) 0.1577(2) 0.0345(7) Uani 1 1 d . . .
H10A H 0.5216 -0.5768 0.1236 0.052 Uiso 1 1 calc R . .
H10B H 0.6614 -0.5293 0.1984 0.052 Uiso 1 1 calc R . .
H10C H 0.6365 -0.4638 0.1190 0.052 Uiso 1 1 calc R . .
C11 C 0.3927(3) -0.5086(3) 0.2762(2) 0.0364(7) Uani 1 1 d . . .
H11A H 0.3418 -0.4639 0.3123 0.055 Uiso 1 1 calc R . .
H11B H 0.4574 -0.5433 0.3127 0.055 Uiso 1 1 calc R . .
H11C H 0.3246 -0.5716 0.2332 0.055 Uiso 1 1 calc R . .
C12 C 0.7483(2) -0.2134(2) 0.12604(15) 0.0179(5) Uani 1 1 d . . .
H12 H 0.6790 -0.2906 0.1030 0.022 Uiso 1 1 calc R . .
C13 C 1.0718(3) -0.1302(3) 0.14701(19) 0.0320(6) Uani 1 1 d . . .
H13A H 1.0600 -0.0602 0.1851 0.048 Uiso 1 1 calc R . .
H13B H 1.0696 -0.1148 0.0886 0.048 Uiso 1 1 calc R . .
H13C H 1.1627 -0.1486 0.1693 0.048 Uiso 1 1 calc R . .
C14 C 0.9257(3) -0.3811(3) 0.05277(19) 0.0347(7) Uani 1 1 d . . .
H14A H 0.9183 -0.3527 -0.0016 0.052 Uiso 1 1 calc R . .
H14B H 0.8452 -0.4466 0.0478 0.052 Uiso 1 1 calc R . .
H14C H 1.0141 -0.4083 0.0649 0.052 Uiso 1 1 calc R . .
C15 C 0.9630(3) -0.3198(2) 0.24333(17) 0.0256(5) Uani 1 1 d . . .
H15A H 1.0537 -0.3439 0.2474 0.038 Uiso 1 1 calc R . .
H15B H 0.8875 -0.3884 0.2405 0.038 Uiso 1 1 calc R . .
H15C H 0.9676 -0.2595 0.2944 0.038 Uiso 1 1 calc R . .
C16 C 0.5240(3) -0.1539(3) -0.01055(17) 0.0274(6) Uani 1 1 d . . .
H16A H 0.4775 -0.1213 0.0343 0.041 Uiso 1 1 calc R . .
H16B H 0.4833 -0.2386 -0.0303 0.041 Uiso 1 1 calc R . .
H16C H 0.5095 -0.1142 -0.0595 0.041 Uiso 1 1 calc R . .
C17 C 0.7995(3) 0.0315(2) 0.06976(18) 0.0280(6) Uani 1 1 d . . .
H17A H 0.7878 0.0690 0.0195 0.042 Uiso 1 1 calc R . .
H17B H 0.9005 0.0428 0.0948 0.042 Uiso 1 1 calc R . .
H17C H 0.7527 0.0673 0.1132 0.042 Uiso 1 1 calc R . .
C18 C 0.7930(3) -0.1877(3) -0.05910(17) 0.0330(6) Uani 1 1 d . . .
H18A H 0.7723 -0.1444 -0.1053 0.049 Uiso 1 1 calc R . .
H18B H 0.7501 -0.2717 -0.0806 0.049 Uiso 1 1 calc R . .
H18C H 0.8957 -0.1770 -0.0406 0.049 Uiso 1 1 calc R . .
C19 C 1.1236(3) 0.2387(2) 0.31794(18) 0.0280(6) Uani 1 1 d . . .
C20 C 0.9203(3) 0.3382(2) 0.22411(18) 0.0313(6) Uani 1 1 d . . .
C21 C 1.0952(3) 0.4730(2) 0.38854(17) 0.0269(6) Uani 1 1 d . . .
C22 C 0.8104(3) 0.4011(2) 0.37878(18) 0.0289(6) Uani 1 1 d . . .
C23 C 1.0112(3) 0.2851(2) 0.47178(17) 0.0240(5) Uani 1 1 d . . .
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'
Si Si 0.0817 0.0704 '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'
W W -0.8490 6.8722 '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'
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 W1 C23 88.96(11) . . ?
C21 W1 C22 85.12(11) . . ?
C23 W1 C22 92.13(11) . . ?
C21 W1 C19 90.74(11) . . ?
C23 W1 C19 89.90(11) . . ?
C22 W1 C19 175.35(11) . . ?
C21 W1 C20 91.32(12) . . ?
C23 W1 C20 177.26(11) . . ?
C22 W1 C20 90.61(12) . . ?
C19 W1 C20 87.37(12) . . ?
C21 W1 P2 178.96(8) . . ?
C23 W1 P2 90.00(8) . . ?
C22 W1 P2 94.82(8) . . ?
C19 W1 P2 89.36(8) . . ?
C20 W1 P2 89.72(9) . . ?
C3 Ge1 C5 115.28(10) . . ?
C3 Ge1 C12 109.73(10) . . ?
C5 Ge1 C12 112.69(10) . . ?
C3 Ge1 P1 97.60(7) . . ?
C5 Ge1 P1 108.64(7) . . ?
C12 Ge1 P1 111.99(7) . . ?
C1 P1 Ge1 96.10(8) . . ?
C3 P2 C1 106.85(12) . . ?
C3 P2 W1 128.08(9) . . ?
C1 P2 W1 124.85(9) . . ?
C7 Si1 C6 106.76(14) . . ?
C7 Si1 C8 109.43(14) . . ?
C6 Si1 C8 105.36(14) . . ?
C7 Si1 C5 111.62(12) . . ?
C6 Si1 C5 113.10(12) . . ?
C8 Si1 C5 110.30(12) . . ?
C11 Si2 C9 107.14(15) . . ?
C11 Si2 C10 103.47(13) . . ?
C9 Si2 C10 108.68(15) . . ?
C11 Si2 C5 113.42(13) . . ?
C9 Si2 C5 110.98(12) . . ?
C10 Si2 C5 112.72(12) . . ?
C13 Si3 C15 109.46(13) . . ?
C13 Si3 C14 108.85(14) . . ?
C15 Si3 C14 104.21(13) . . ?
C13 Si3 C12 110.48(12) . . ?
C15 Si3 C12 113.47(12) . . ?
C14 Si3 C12 110.12(13) . . ?
C16 Si4 C17 110.23(13) . . ?
C16 Si4 C18 104.41(13) . . ?
C17 Si4 C18 106.98(14) . . ?
C16 Si4 C12 110.01(12) . . ?
C17 Si4 C12 112.84(12) . . ?
C18 Si4 C12 112.01(12) . . ?
C2 C1 P1 120.13(18) . . ?
C2 C1 P2 115.76(19) . . ?
P1 C1 P2 124.09(14) . . ?
C4 C3 P2 120.72(18) . . ?
C4 C3 Ge1 125.03(17) . . ?
P2 C3 Ge1 114.25(12) . . ?
Si1 C5 Si2 114.06(13) . . ?
Si1 C5 Ge1 114.17(12) . . ?
Si2 C5 Ge1 111.75(12) . . ?
Si3 C12 Si4 114.55(13) . . ?
Si3 C12 Ge1 115.27(12) . . ?
Si4 C12 Ge1 115.31(12) . . ?
O1 C19 W1 178.8(3) . . ?
O2 C20 W1 178.6(3) . . ?
O3 C21 W1 177.7(2) . . ?
O4 C22 W1 175.1(3) . . ?
O5 C23 W1 177.5(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
W1 C21 2.010(3) . ?
W1 C23 2.036(3) . ?
W1 C22 2.044(3) . ?
W1 C19 2.048(3) . ?
W1 C20 2.054(3) . ?
W1 P2 2.4848(12) . ?
Ge1 C3 1.975(3) . ?
Ge1 C5 1.989(2) . ?
Ge1 C12 1.994(2) . ?
Ge1 P1 2.3403(9) . ?
P1 C1 1.691(3) . ?
P2 C3 1.674(2) . ?
P2 C1 1.813(2) . ?
Si1 C7 1.870(3) . ?
Si1 C6 1.877(3) . ?
Si1 C8 1.878(3) . ?
Si1 C5 1.900(3) . ?
Si2 C11 1.871(3) . ?
Si2 C9 1.872(3) . ?
Si2 C10 1.878(3) . ?
Si2 C5 1.900(3) . ?
Si3 C13 1.869(3) . ?
Si3 C15 1.874(3) . ?
Si3 C14 1.877(3) . ?
Si3 C12 1.894(2) . ?
Si4 C16 1.872(3) . ?
Si4 C17 1.873(3) . ?
Si4 C18 1.875(3) . ?
Si4 C12 1.898(2) . ?
O1 C19 1.135(3) . ?
O2 C20 1.137(3) . ?
O3 C21 1.145(3) . ?
O4 C22 1.137(3) . ?
O5 C23 1.140(3) . ?
C1 C2 1.513(3) . ?
C3 C4 1.503(3) . ?
