#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:45:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178666 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/77/4077755.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_4077755
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            'C17 H27 O8 P W2'
_chemical_formula_weight         758.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 94.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.201(2)
_cell_length_b                   10.034(2)
_cell_length_c                   20.883(4)
_cell_measurement_reflns_used    1257
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      1.96
_cell_volume                     2547.4(8)
_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  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'STOE IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_av_sigmaI/netI    0.1157
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9022
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    9.120
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_description       Route
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.854
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_obs          0.0482
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0254P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0988
_refine_ls_wR_factor_obs         0.0853
_reflns_number_observed          2528
_reflns_number_total             4107
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990019e.cif
_cod_data_source_block           pwob
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+0.0000P] 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^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2547.4(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077755
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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 0.39977(5) 0.23406(7) 0.08408(2) 0.0351(2) Uani 1 d .
W2 W 0.12581(5) 0.40900(7) 0.19734(2) 0.0299(2) Uani 1 d .
P P 0.2558(3) 0.3217(4) 0.14954(15) 0.0345(9) Uani 1 d .
C1 C 0.2871(14) 0.1101(20) 0.0385(5) 0.046(5) Uani 1 d .
O1 O 0.2180(11) 0.0428(16) 0.0147(6) 0.069(4) Uani 1 d .
C2 C 0.4372(14) 0.0801(25) 0.1481(8) 0.057(5) Uani 1 d .
O2 O 0.4583(12) -0.0003(17) 0.1831(6) 0.081(5) Uani 1 d .
C3 C 0.5085(15) 0.3573(23) 0.1346(6) 0.057(5) Uani 1 d .
O3 O 0.5714(11) 0.4235(18) 0.1625(5) 0.076(5) Uani 1 d .
C4 C 0.3667(14) 0.3827(27) 0.0178(6) 0.064(7) Uani 1 d .
O4 O 0.3533(13) 0.4678(18) -0.0186(5) 0.082(5) Uani 1 d .
C5 C 0.5134(16) 0.1727(18) 0.0276(7) 0.050(4) Uani 1 d .
O5 O 0.5780(13) 0.1385(19) -0.0061(7) 0.094(5) Uani 1 d .
O6 O 0.1459(8) 0.5941(13) 0.1966(4) 0.040(2) Uani 1 d .
O7 O -0.0055(8) 0.3620(11) 0.1536(4) 0.035(2) Uani 1 d .
O8 O 0.1338(8) 0.3457(10) 0.2805(4) 0.032(2) Uani 1 d .
C6 C 0.2247(14) 0.6940(17) 0.1802(6) 0.039(4) Uani 1 d .
C7 C 0.1751(17) 0.8292(20) 0.2001(8) 0.058(5) Uani 1 d .
H7A H 0.1045(41) 0.8439(53) 0.1752(37) 0.087 Uiso 1 calc R
H7B H 0.2258(39) 0.9016(23) 0.1916(46) 0.087 Uiso 1 calc R
H7C H 0.1639(84) 0.8272(43) 0.2460(14) 0.087 Uiso 1 calc R
C8 C 0.3298(16) 0.6677(28) 0.2210(9) 0.074(6) Uani 1 d .
H8A H 0.3642(63) 0.5864(74) 0.2060(45) 0.111 Uiso 1 calc R
H8B H 0.3139(21) 0.6565(154) 0.2659(14) 0.111 Uiso 1 calc R
H8C H 0.3801(47) 0.7431(60) 0.2176(54) 0.111 Uiso 1 calc R
C9 C 0.2378(20) 0.6865(23) 0.1089(7) 0.076(7) Uani 1 d .
H9A H 0.2533(142) 0.5943(38) 0.0971(17) 0.114 Uiso 1 calc R
H9B H 0.2989(99) 0.7439(138) 0.0986(16) 0.114 Uiso 1 calc R
H9C H 0.1698(58) 0.7165(169) 0.0849(8) 0.114 Uiso 1 calc R
C10 C -0.0517(12) 0.2675(17) 0.1018(5) 0.037(4) Uani 1 d .
C11 C -0.1747(15) 0.2950(30) 0.0964(8) 0.077(8) Uani 1 d .
H11A H -0.2117(21) 0.2346(95) 0.0646(55) 0.116 Uiso 1 calc R
H11B H -0.1881(17) 0.3875(43) 0.0828(69) 0.116 Uiso 1 calc R
H11C H -0.2035(26) 0.2805(159) 0.1382(21) 0.116 Uiso 1 calc R
C12 C -0.0194(24) 0.1298(29) 0.1225(9) 0.097(9) Uani 1 d .
H12A H 0.0599(26) 0.1270(48) 0.1348(74) 0.145 Uiso 1 calc R
H12B H -0.0375(135) 0.0676(37) 0.0871(29) 0.145 Uiso 1 calc R
H12C H -0.0594(95) 0.1044(68) 0.1594(52) 0.145 Uiso 1 calc R
C13 C 0.0000(18) 0.2987(31) 0.0406(7) 0.091(10) Uani 1 d .
H13A H 0.0802(20) 0.2922(193) 0.0481(25) 0.137 Uiso 1 calc R
H13B H -0.0204(124) 0.3892(68) 0.0265(48) 0.137 Uiso 1 calc R
H13C H -0.0263(124) 0.2349(112) 0.0072(27) 0.137 Uiso 1 calc R
C14 C 0.1968(13) 0.2636(17) 0.3270(5) 0.038(4) Uani 1 d .
C15 C 0.1268(15) 0.2444(23) 0.3841(6) 0.056(5) Uani 1 d .
H15A H 0.1631(56) 0.1805(92) 0.4144(30) 0.084 Uiso 1 calc R
H15B H 0.0541(41) 0.2103(125) 0.3686(9) 0.084 Uiso 1 calc R
H15C H 0.1186(84) 0.3300(28) 0.4058(36) 0.084 Uiso 1 calc R
C16 C 0.2077(21) 0.1245(28) 0.2951(8) 0.090(9) Uani 1 d .
H16A H 0.2367(123) 0.0602(47) 0.3275(17) 0.135 Uiso 1 calc R
H16B H 0.2579(92) 0.1308(46) 0.2610(49) 0.135 Uiso 1 calc R
H16C H 0.1352(25) 0.0948(68) 0.2767(63) 0.135 Uiso 1 calc R
C17 C 0.3035(18) 0.3307(36) 0.3462(9) 0.107(12) Uani 1 d .
H17A H 0.3524(58) 0.2685(56) 0.3709(82) 0.160 Uiso 1 calc R
H17B H 0.2904(22) 0.4088(104) 0.3728(84) 0.160 Uiso 1 calc R
H17C H 0.3377(87) 0.3591(200) 0.3077(10) 0.160 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
C5 W1 C1 90.6(6)
C5 W1 C3 92.2(7)
C1 W1 C3 176.7(5)
C5 W1 C4 86.1(7)
C1 W1 C4 92.4(7)
C3 W1 C4 89.5(7)
C5 W1 C2 91.5(7)
C1 W1 C2 87.1(7)
C3 W1 C2 91.1(7)
C4 W1 C2 177.5(7)
C5 W1 P 176.5(5)
C1 W1 P 89.6(4)
C3 W1 P 87.7(5)
C4 W1 P 90.4(5)
C2 W1 P 92.1(5)
O7 W2 O8 110.7(4)
O7 W2 O6 111.1(4)
O8 W2 O6 110.7(4)
O7 W2 P 108.3(3)
O8 W2 P 108.5(3)
O6 W2 P 107.5(3)
W2 P W1 174.0(2)
O1 C1 W1 175.7(12)
O2 C2 W1 178.6(20)
O3 C3 W1 178.0(20)
O4 C4 W1 176.8(16)
O5 C5 W1 178.6(18)
C6 O6 W2 141.0(10)
C10 O7 W2 140.7(9)
C14 O8 W2 144.3(8)
O6 C6 C8 107.2(14)
O6 C6 C9 109.0(12)
C8 C6 C9 113.1(17)
O6 C6 C7 105.1(13)
C8 C6 C7 109.5(15)
C9 C6 C7 112.5(14)
C12 C10 C13 108.7(19)
C12 C10 O7 107.4(12)
C13 C10 O7 108.7(14)
C12 C10 C11 115.1(19)
C13 C10 C11 112.4(15)
O7 C10 C11 104.2(14)
O8 C14 C17 109.1(15)
O8 C14 C15 107.1(13)
C17 C14 C15 112.2(14)
O8 C14 C16 106.4(11)
C17 C14 C16 114.6(19)
C15 C14 C16 107.0(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 C5 1.991(15)
W1 C1 2.03(2)
W1 C3 2.04(2)
W1 C4 2.05(2)
W1 C2 2.07(2)
W1 P 2.476(4)
W2 O7 1.837(9)
W2 O8 1.844(8)
W2 O6 1.874(13)
W2 P 2.132(4)
C1 O1 1.16(2)
C2 O2 1.10(2)
C3 O3 1.14(2)
C4 O4 1.15(3)
C5 O5 1.15(2)
O6 C6 1.45(2)
O7 C10 1.512(15)
O8 C14 1.44(2)
C6 C8 1.50(2)
C6 C9 1.51(2)
C6 C7 1.56(3)
C10 C12 1.49(3)
C10 C13 1.50(2)
C10 C11 1.52(2)
C14 C17 1.49(3)
C14 C15 1.54(2)
C14 C16 1.56(3)
