#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:45:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178666 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/77/4077753.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_4077753
loop_
_publ_author_name
'Scheer, Manfred'
'Kramkowski, Peter'
'Schuster, Kay'
_publ_section_title
;
 An Approach to Novel Complexes with a Tungsten−Phosphorus Triple
 Bond†
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              2874
_journal_paper_doi               10.1021/om990019e
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C34 H57 O3 P W'
_chemical_formula_weight         728.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1410(10)
_cell_length_b                   10.9600(10)
_cell_length_c                   31.183(4)
_cell_measurement_reflns_used    1211
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      4.95
_cell_volume                     3465.8(6)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software'
_computing_molecular_graphics    SIEMENS-XP
_computing_publication_material  SKHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(1)
_diffrn_measurement_device       'STOE IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            20993
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         4.95
_exptl_absorpt_coefficient_mu    3.409
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.225
_refine_diff_density_min         -1.658
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.107
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_obs          0.0504
_refine_ls_shift/esd_max         0.944
_refine_ls_shift/esd_mean        0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0381P)²+22.8504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1259
_refine_ls_wR_factor_obs         0.1167
_reflns_number_observed          7506
_reflns_number_total             8296
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990019e.cif
_cod_data_source_block           ad1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+22.8504P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+22.8504P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4077753
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W 0.16541(3) 0.36259(3) 0.108842(10) 0.03277(9) Uani 1 d .
P1 P 0.3598(2) 0.2227(2) 0.12235(7) 0.0329(4) Uani 1 d .
O1 O 0.0785(7) 0.4352(7) 0.1557(2) 0.045(2) Uani 1 d .
O2 O 0.0840(8) 0.4190(7) 0.0594(2) 0.051(2) Uani 1 d .
O3 O 0.3844(7) 0.2147(7) 0.1756(2) 0.055(2) Uani 1 d .
C1 C 0.1756(10) 0.1929(7) 0.1144(2) 0.034(2) Uani 1 d .
C2 C 0.3547(5) 0.3815(5) 0.1098(2) 0.0230(12) Uani 1 d .
C3 C 0.0648(11) 0.4387(10) 0.2026(3) 0.048(2) Uani 1 d .
C4 C -0.0319(27) 0.5298(22) 0.2127(6) 0.146(12) Uani 1 d .
H4A H -0.0504(152) 0.5780(123) 0.1873(18) 0.220 Uiso 1 calc R
H4B H 0.0015(81) 0.5825(113) 0.2352(46) 0.220 Uiso 1 calc R
H4C H -0.1123(69) 0.4905(22) 0.2223(61) 0.220 Uiso 1 calc R
C5 C 0.0448(49) 0.3210(18) 0.2184(6) 0.274(27) Uani 1 d .
H5A H -0.0488(52) 0.3069(154) 0.2223(143) 0.411 Uiso 1 calc R
H5B H 0.0895(385) 0.3123(137) 0.2458(74) 0.411 Uiso 1 calc R
H5C H 0.0800(434) 0.2621(24) 0.1982(73) 0.411 Uiso 1 calc R
C6 C 0.1946(22) 0.4892(33) 0.2180(5) 0.189(14) Uani 1 d .
H6A H 0.1863(80) 0.5146(244) 0.2477(28) 0.283 Uiso 1 calc R
H6B H 0.2190(133) 0.5588(149) 0.2005(57) 0.283 Uiso 1 calc R
H6C H 0.2620(63) 0.4268(76) 0.2157(82) 0.283 Uiso 1 calc R
C7 C 0.0626(10) 0.4224(9) 0.0147(3) 0.042(2) Uani 1 d .
C8 C 0.0326(21) 0.5510(12) 0.0030(5) 0.094(6) Uani 1 d .
H8A H -0.0056(114) 0.5535(16) -0.0255(17) 0.142 Uiso 1 calc R
H8B H 0.1133(28) 0.5985(27) 0.0034(38) 0.142 Uiso 1 calc R
H8C H -0.0294(95) 0.5848(37) 0.0235(24) 0.142 Uiso 1 calc R
C9 C -0.0560(12) 0.3405(13) 0.0050(5) 0.071(4) Uani 1 d .
H9A H -0.0743(61) 0.3421(70) -0.0255(6) 0.106 Uiso 1 calc R
H9B H -0.1324(26) 0.3699(54) 0.0206(25) 0.106 Uiso 1 calc R
H9C H -0.0364(38) 0.2575(21) 0.0138(29) 0.106 Uiso 1 calc R
C10 C 0.1804(13) 0.3689(15) -0.0078(4) 0.076(3) Uani 1 d .
H10A H 0.1598(39) 0.3567(96) -0.0379(8) 0.115 Uiso 1 calc R
H10B H 0.2027(67) 0.2912(50) 0.0052(23) 0.115 Uiso 1 calc R
H10C H 0.2545(33) 0.4243(48) -0.0052(31) 0.115 Uiso 1 calc R
C11 C 0.1221(7) 0.0668(7) 0.1113(3) 0.034(2) Uani 1 d .
C12 C 0.1371(10) 0.0031(10) 0.1557(3) 0.049(2) Uani 1 d .
H12A H 0.2307(10) -0.0094(10) 0.1621(3) 0.059 Uiso 1 calc R
H12B H 0.0995(10) 0.0550(10) 0.1782(3) 0.059 Uiso 1 calc R
C13 C 0.1771(13) -0.0105(9) 0.0765(4) 0.055(2) Uani 1 d .
H13A H 0.2719(13) -0.0222(9) 0.0809(4) 0.065 Uiso 1 calc R
H13B H 0.1643(13) 0.0296(9) 0.0487(4) 0.065 Uiso 1 calc R
C14 C -0.0315(9) 0.0865(9) 0.1044(4) 0.049(2) Uani 1 d .
H14A H -0.0679(9) 0.1355(9) 0.1279(4) 0.059 Uiso 1 calc R
H14B H -0.0473(9) 0.1296(9) 0.0774(4) 0.059 Uiso 1 calc R
C15 C -0.0980(11) -0.0395(10) 0.1034(4) 0.055(3) Uani 1 d .
H15 H -0.1935(11) -0.0285(10) 0.0982(4) 0.066 Uiso 1 calc R
C16 C -0.0418(14) -0.1152(12) 0.0685(4) 0.072(4) Uani 1 d .
H16A H -0.0540(14) -0.0740(12) 0.0409(4) 0.086 Uiso 1 calc R
H16B H -0.0876(14) -0.1939(12) 0.0673(4) 0.086 Uiso 1 calc R
C17 C 0.1058(13) -0.1359(13) 0.0768(4) 0.071(4) Uani 1 d .
H17 H 0.1426(13) -0.1882(13) 0.0538(4) 0.085 Uiso 1 calc R
C18 C 0.1246(14) -0.1970(10) 0.1190(5) 0.072(4) Uani 1 d .
H18A H 0.2190(14) -0.2091(10) 0.1243(5) 0.086 Uiso 1 calc R
H18B H 0.0821(14) -0.2772(10) 0.1186(5) 0.086 Uiso 1 calc R
C19 C 0.0657(12) -0.1200(9) 0.1550(4) 0.053(3) Uani 1 d .
H19 H 0.0791(12) -0.1620(9) 0.1828(4) 0.064 Uiso 1 calc R
C20 C -0.0786(12) -0.1007(11) 0.1477(4) 0.059(3) Uani 1 d .
H20A H -0.1149(12) -0.0484(11) 0.1703(4) 0.071 Uiso 1 calc R
H20B H -0.1250(12) -0.1791(11) 0.1485(4) 0.071 Uiso 1 calc R
C21 C 0.4580(8) 0.4742(7) 0.1035(3) 0.035(2) Uani 1 d .
C22 C 0.5674(16) 0.4327(18) 0.0757(8) 0.126(9) Uani 1 d .
H22A H 0.5315(16) 0.3958(18) 0.0496(8) 0.151 Uiso 1 calc R
H22B H 0.6191(16) 0.3705(18) 0.0908(8) 0.151 Uiso 1 calc R
C23 C 0.5159(22) 0.5128(19) 0.1464(4) 0.122(8) Uani 1 d .
H23A H 0.5468(22) 0.4407(19) 0.1620(4) 0.146 Uiso 1 calc R
H23B H 0.4476(22) 0.5526(19) 0.1637(4) 0.146 Uiso 1 calc R
C24 C 0.4034(17) 0.5869(17) 0.0845(10) 0.169(13) Uani 1 d .
H24A H 0.3213(17) 0.6088(17) 0.0992(10) 0.202 Uiso 1 calc R
H24B H 0.3830(17) 0.5730(17) 0.0541(10) 0.202 Uiso 1 calc R
C25 C 0.6351(22) 0.6042(17) 0.1392(4) 0.114(8) Uani 1 d .
H25 H 0.6818(22) 0.6160(17) 0.1667(4) 0.137 Uiso 1 calc R
C26 C 0.7307(14) 0.5534(18) 0.1066(10) 0.137(10) Uani 1 d .
H26A H 0.7575(14) 0.4709(18) 0.1150(10) 0.165 Uiso 1 calc R
H26B H 0.8097(14) 0.6047(18) 0.1055(10) 0.165 Uiso 1 calc R
C27 C 0.6653(17) 0.5497(21) 0.0626(7) 0.130(9) Uani 1 d .
H27 H 0.7270(17) 0.5317(21) 0.0388(7) 0.156 Uiso 1 calc R
C28 C 0.5791(29) 0.6556(19) 0.0546(7) 0.123(9) Uani 1 d .
H28A H 0.6331(29) 0.7209(19) 0.0422(7) 0.147 Uiso 1 calc R
H28B H 0.5139(29) 0.6322(19) 0.0329(7) 0.147 Uiso 1 calc R
C29 C 0.5128(25) 0.7025(19) 0.0890(10) 0.120(8) Uani 1 d .
H29 H 0.4708(25) 0.7809(19) 0.0813(10) 0.144 Uiso 1 calc R
C30 C 0.5764(19) 0.7125(20) 0.1275(12) 0.157(14) Uani 1 d .
H30A H 0.5130(19) 0.7368(20) 0.1496(12) 0.188 Uiso 1 calc R
H30B H 0.6438(19) 0.7763(20) 0.1255(12) 0.188 Uiso 1 calc R
C31 C 0.4881(13) 0.1490(11) 0.1979(4) 0.063(3) Uani 1 d .
C32 C 0.5520(38) 0.0647(38) 0.1705(8) 0.285(29) Uani 1 d .
H32A H 0.5986(406) 0.1087(42) 0.1482(94) 0.427 Uiso 1 calc R
H32B H 0.4869(58) 0.0113(293) 0.1576(121) 0.427 Uiso 1 calc R
H32C H 0.6142(355) 0.0165(306) 0.1870(30) 0.427 Uiso 1 calc R
C33 C 0.5719(33) 0.2392(22) 0.2184(13) 0.253(25) Uani 1 d .
H33A H 0.5940(337) 0.2122(184) 0.2471(48) 0.380 Uiso 1 calc R
H33B H 0.5257(158) 0.3166(105) 0.2199(123) 0.380 Uiso 1 calc R
H33C H 0.6521(186) 0.2491(276) 0.2018(72) 0.380 Uiso 1 calc R
C34 C 0.4288(30) 0.0782(37) 0.2318(11) 0.243(22) Uani 1 d .
H34A H 0.3358(88) 0.0668(296) 0.2258(62) 0.364 Uiso 1 calc R
H34B H 0.4390(322) 0.1209(160) 0.2589(23) 0.364 Uiso 1 calc R
H34C H 0.4718(251) -0.0006(132) 0.2336(79) 0.364 Uiso 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'
P P 0.1023 0.0942 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O2 W1 C1 115.6(3)
O2 W1 O1 107.2(3)
C1 W1 O1 112.0(3)
O2 W1 C2 114.8(3)
C1 W1 C2 92.9(3)
O1 W1 C2 114.1(3)
O2 W1 P1 133.3(2)
C1 W1 P1 48.7(3)
O1 W1 P1 119.5(2)
C2 W1 P1 44.7(2)
O3 P1 C2 105.8(4)
O3 P1 C1 105.3(3)
C2 P1 C1 96.3(3)
O3 P1 W1 108.2(3)
C2 P1 W1 49.5(2)
C1 P1 W1 47.3(2)
C3 O1 W1 145.8(7)
C7 O2 W1 154.0(7)
C31 O3 P1 127.5(8)
C11 C1 W1 153.8(7)
C11 C1 P1 121.6(6)
W1 C1 P1 84.0(3)
C21 C2 P1 132.9(5)
C21 C2 W1 141.2(5)
P1 C2 W1 85.8(2)
C5 C3 C4 117.9(22)
C5 C3 O1 109.9(10)
C4 C3 O1 107.4(10)
C5 C3 C6 110.7(26)
C4 C3 C6 105.8(19)
O1 C3 C6 104.1(10)
O2 C7 C8 107.4(10)
O2 C7 C10 109.1(9)
C8 C7 C10 114.7(12)
O2 C7 C9 107.5(9)
C8 C7 C9 110.3(11)
C10 C7 C9 107.6(10)
C13 C11 C1 116.1(8)
C13 C11 C12 110.9(8)
C1 C11 C12 108.9(7)
C13 C11 C14 110.3(8)
C1 C11 C14 103.9(7)
C12 C11 C14 106.1(8)
C19 C12 C11 109.7(8)
C11 C13 C17 109.0(9)
C15 C14 C11 108.2(8)
C16 C15 C14 110.5(9)
C16 C15 C20 111.3(10)
C14 C15 C20 108.3(9)
C15 C16 C17 109.6(10)
C18 C17 C16 109.8(10)
C18 C17 C13 110.0(11)
C16 C17 C13 108.8(12)
C17 C18 C19 110.6(10)
C20 C19 C18 110.5(10)
C20 C19 C12 109.8(9)
C18 C19 C12 108.2(9)
C19 C20 C15 108.7(9)
C2 C21 C22 113.6(9)
C2 C21 C24 111.3(8)
C22 C21 C24 107.7(17)
C2 C21 C23 110.4(8)
C22 C21 C23 108.1(14)
C24 C21 C23 105.3(15)
C21 C22 C27 110.7(12)
C21 C23 C25 110.2(10)
C21 C24 C29 110.3(12)
C30 C25 C26 114.6(18)
C30 C25 C23 104.6(19)
C26 C25 C23 110.6(14)
C25 C26 C27 109.6(13)
C28 C27 C26 112.9(14)
C28 C27 C22 107.0(15)
C26 C27 C22 93.3(18)
C29 C28 C27 117.1(17)
C28 C29 C30 119.2(23)
C28 C29 C24 88.6(22)
C30 C29 C24 116.3(18)
C29 C30 C25 111.5(16)
C32 C31 C34 106.4(28)
C32 C31 C33 116.2(27)
C34 C31 C33 106.8(25)
C32 C31 O3 111.3(12)
C34 C31 O3 108.5(15)
C33 C31 O3 107.3(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 O2 1.855(7)
W1 C1 1.871(8)
W1 O1 1.883(7)
W1 C2 1.931(5)
W1 P1 2.533(2)
P1 O3 1.680(8)
P1 C2 1.785(6)
P1 C1 1.913(10)
O1 C3 1.472(12)
O2 C7 1.412(11)
O3 C31 1.452(13)
C1 C11 1.488(10)
C2 C21 1.472(9)
C3 C5 1.40(2)
C3 C4 1.43(2)
C3 C6 1.51(2)
C7 C8 1.49(2)
C7 C10 1.504(15)
C7 C9 1.53(2)
C11 C13 1.486(13)
C11 C12 1.558(12)
C11 C14 1.586(12)
C12 C19 1.531(14)
C13 C17 1.55(2)
C14 C15 1.537(12)
C15 C16 1.48(2)
C15 C20 1.55(2)
C16 C17 1.54(2)
C17 C18 1.49(2)
C18 C19 1.53(2)
C19 C20 1.50(2)
C21 C22 1.48(2)
C21 C24 1.48(2)
C21 C23 1.521(15)
C22 C27 1.67(3)
C23 C25 1.59(2)
C24 C29 1.69(3)
C25 C30 1.38(3)
C25 C26 1.51(3)
C26 C27 1.52(3)
C27 C28 1.47(3)
C28 C29 1.37(3)
C29 C30 1.37(3)
C31 C32 1.42(3)
C31 C34 1.44(3)
C31 C33 1.45(2)
