#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/06/7050638.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_7050638
loop_
_publ_author_name
'Brym, Markus'
'Jones, Cameron'
'Waugh, Mark'
'Hey-Hawkins, Evamarie'
'Majoumo, Felecite'
_publ_section_title
;
 Reactions of phosphavinyl Grignard reagents with aldehydes: synthesis,
 characterisation and further reactivity of ?-phosphaallylic alcohols
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1614
_journal_paper_doi               10.1039/b306607j
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C30 H42 O8 P2 W2'
_chemical_formula_weight         960.28
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 125.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.598(5)
_cell_length_b                   9.4670(19)
_cell_length_c                   17.439(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3426.8(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1137
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27823
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    6.846
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.391
_refine_diff_density_min         -2.376
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0429P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                3013
_reflns_number_total             3935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306607j.txt
_cod_data_source_block           compound_9
_cod_original_cell_volume        3426.8(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050638
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
W1 W 0.053359(10) 0.71807(2) 0.392936(16) 0.01893(9) Uani 1 1 d . . .
P1 P 0.06227(7) 0.69927(15) 0.25403(11) 0.0187(3) Uani 1 1 d . . .
O1 O 0.1953(2) 0.7292(6) 0.5740(4) 0.0474(13) Uani 1 1 d . . .
C1 C 0.0850(3) 0.5453(6) 0.3219(4) 0.0201(12) Uani 1 1 d . . .
O2 O 0.0573(3) 1.0472(5) 0.3612(4) 0.0512(14) Uani 1 1 d . . .
C2 C 0.1469(3) 0.4553(6) 0.3757(4) 0.0274(14) Uani 1 1 d . . .
O3 O 0.0234(2) 0.8469(5) 0.5300(3) 0.0385(11) Uani 1 1 d . . .
C3 C 0.2099(3) 0.5356(7) 0.4177(5) 0.0321(15) Uani 1 1 d . . .
H3A H 0.2131 0.6121 0.4581 0.048 Uiso 1 1 calc R . .
H3B H 0.2107 0.5754 0.3665 0.048 Uiso 1 1 calc R . .
H3C H 0.2463 0.4708 0.4555 0.048 Uiso 1 1 calc R . .
O4 O 0.0211(2) 0.4257(5) 0.4463(4) 0.0470(13) Uani 1 1 d . . .
C4 C 0.1394(3) 0.3477(7) 0.3039(5) 0.0381(16) Uani 1 1 d . . .
H4A H 0.1794 0.2938 0.3326 0.057 Uiso 1 1 calc R . .
H4B H 0.1300 0.3975 0.2479 0.057 Uiso 1 1 calc R . .
H4C H 0.1039 0.2830 0.2854 0.057 Uiso 1 1 calc R . .
C5 C 0.1522(3) 0.3722(7) 0.4552(5) 0.0369(16) Uani 1 1 d . . .
H5A H 0.1114 0.3232 0.4301 0.055 Uiso 1 1 calc R . .
H5B H 0.1613 0.4374 0.5054 0.055 Uiso 1 1 calc R . .
H5C H 0.1870 0.3029 0.4810 0.055 Uiso 1 1 calc R . .
C6 C 0.1293(3) 0.7862(6) 0.2596(4) 0.0218(12) Uani 1 1 d . . .
H6 H 0.1696 0.7770 0.3252 0.026 Uiso 1 1 calc R . .
C7 C 0.1150(3) 0.9442(6) 0.2341(5) 0.0275(14) Uani 1 1 d . . .
H7A H 0.0720 0.9546 0.1732 0.033 Uiso 1 1 calc R . .
H7B H 0.1142 0.9938 0.2834 0.033 Uiso 1 1 calc R . .
C8 C 0.1662(3) 1.0126(7) 0.2261(5) 0.0336(16) Uani 1 1 d . . .
H8A H 0.1539 1.1119 0.2053 0.040 Uiso 1 1 calc R . .
H8B H 0.2081 1.0131 0.2892 0.040 Uiso 1 1 calc R . .
C9 C 0.1735(3) 0.9360(7) 0.1575(5) 0.0353(16) Uani 1 1 d . . .
H9A H 0.2080 0.9814 0.1565 0.042 Uiso 1 1 calc R . .
H9B H 0.1328 0.9429 0.0932 0.042 Uiso 1 1 calc R . .
C10 C 0.1902(3) 0.7803(7) 0.1847(5) 0.0319(15) Uani 1 1 d . . .
H10A H 0.2327 0.7730 0.2466 0.038 Uiso 1 1 calc R . .
H10B H 0.1931 0.7315 0.1370 0.038 Uiso 1 1 calc R . .
C11 C 0.1386(3) 0.7084(6) 0.1904(4) 0.0241(13) Uani 1 1 d . . .
H11A H 0.1514 0.6094 0.2115 0.029 Uiso 1 1 calc R . .
H11B H 0.0971 0.7069 0.1266 0.029 Uiso 1 1 calc R . .
C12 C 0.1448(3) 0.7270(7) 0.5060(5) 0.0306(15) Uani 1 1 d . . .
C13 C 0.0564(3) 0.9282(7) 0.3681(5) 0.0305(15) Uani 1 1 d . . .
C14 C 0.0322(3) 0.7974(6) 0.4788(5) 0.0243(13) Uani 1 1 d . . .
C15 C 0.0353(3) 0.5269(7) 0.4291(5) 0.0299(15) Uani 1 1 d . . .
H1 H 0.049(3) 0.476(6) 0.289(4) 0.024(15) Uiso 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 W1 C14 85.4(3) . . ?
C12 W1 C13 90.0(3) . . ?
C14 W1 C13 81.7(2) . . ?
C12 W1 C15 94.5(3) . . ?
C14 W1 C15 83.9(2) . . ?
C13 W1 C15 164.4(2) . . ?
C12 W1 C1 89.1(2) . . ?
C14 W1 C1 159.2(2) . . ?
C13 W1 C1 118.4(2) . . ?
C15 W1 C1 76.6(2) . . ?
C12 W1 P1 177.84(19) . 2 ?
C14 W1 P1 96.57(19) . 2 ?
C13 W1 P1 91.18(19) . 2 ?
C15 W1 P1 84.82(18) . 2 ?
C1 W1 P1 88.75(14) . 2 ?
C12 W1 P1 103.60(19) . . ?
C14 W1 P1 159.86(17) . . ?
C13 W1 P1 80.36(18) . . ?
C15 W1 P1 112.85(17) . . ?
C1 W1 P1 40.64(13) . . ?
P1 W1 P1 74.84(6) 2 . ?
C1 P1 C6 113.8(3) . . ?
C1 P1 W1 118.0(2) . 2 ?
C6 P1 W1 121.1(2) . 2 ?
C1 P1 W1 66.25(19) . . ?
C6 P1 W1 120.7(2) . . ?
W1 P1 W1 104.59(6) 2 . ?
C2 C1 P1 133.5(4) . . ?
C2 C1 W1 125.9(4) . . ?
P1 C1 W1 73.1(2) . . ?
C3 C2 C5 108.2(5) . . ?
C3 C2 C4 108.4(5) . . ?
C5 C2 C4 107.4(5) . . ?
C3 C2 C1 116.0(5) . . ?
C5 C2 C1 110.4(5) . . ?
C4 C2 C1 106.1(5) . . ?
C7 C6 C11 110.9(5) . . ?
C7 C6 P1 111.1(4) . . ?
C11 C6 P1 108.0(4) . . ?
C8 C7 C6 111.3(5) . . ?
C9 C8 C7 112.3(5) . . ?
C8 C9 C10 111.2(5) . . ?
C9 C10 C11 110.5(5) . . ?
C10 C11 C6 111.7(5) . . ?
O1 C12 W1 175.2(6) . . ?
O2 C13 W1 173.2(6) . . ?
O3 C14 W1 176.0(5) . . ?
O4 C15 W1 175.0(5) . . ?
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 C12 1.993(7) . ?
W1 C14 2.012(6) . ?
W1 C13 2.047(6) . ?
W1 C15 2.056(7) . ?
W1 C1 2.457(6) . ?
W1 P1 2.546(2) 2 ?
W1 P1 2.5689(16) . ?
P1 C1 1.749(6) . ?
P1 C6 1.854(6) . ?
P1 W1 2.546(2) 2 ?
O1 C12 1.133(8) . ?
C1 C2 1.542(8) . ?
O2 C13 1.135(7) . ?
C2 C3 1.526(8) . ?
C2 C5 1.531(8) . ?
C2 C4 1.536(9) . ?
O3 C14 1.141(7) . ?
O4 C15 1.127(7) . ?
C6 C7 1.543(8) . ?
C6 C11 1.546(8) . ?
C7 C8 1.538(8) . ?
C8 C9 1.501(8) . ?
C9 C10 1.530(9) . ?
C10 C11 1.542(8) . ?
