#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:48:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178535 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/41/4064129.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_4064129
loop_
_publ_author_name
'Tran Huy, Ngoc Hoa'
'Lu, Yunpeng'
'Mathey, François'
_publ_section_title
;
 Oligomerization of Terminal Phosphinidene Complexes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1734
_journal_paper_doi               10.1021/om101144n
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C25 H12 N2 O15 P2 W3'
_chemical_formula_sum            'C25 H12 N2 O15 P2 W3'
_chemical_formula_weight         1193.86
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.847(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8633(5)
_cell_length_b                   21.0617(8)
_cell_length_c                   12.6050(5)
_cell_measurement_reflns_used    6080
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      3.01
_cell_volume                     3145.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            43554
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    11.119
_exptl_absorpt_correction_T_max  0.6647
_exptl_absorpt_correction_T_min  0.4027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.427
_refine_diff_density_min         -2.631
_refine_diff_density_rms         0.501
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0602P)²+28.1653P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                6407
_reflns_number_total             7603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101144n_si_003.cif
_cod_data_source_block           mat33
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4064129
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
W1 W 0.28357(3) 0.080358(16) 0.52610(3) 0.01712(10) Uani 1 1 d .
W2 W 0.19355(3) 0.139744(16) 1.02188(3) 0.01807(10) Uani 1 1 d .
W3 W 0.22767(3) 0.253688(14) 0.72170(2) 0.01152(9) Uani 1 1 d .
C1 C 0.0555(9) 0.1131(4) 0.7156(8) 0.026(2) Uani 1 1 d .
C2 C -0.0451(9) 0.1454(5) 0.6875(9) 0.030(2) Uani 1 1 d .
H2 H -0.0505 0.1886 0.6660 0.036 Uiso 1 1 calc R
C3 C -0.1363(8) 0.1038(5) 0.6964(7) 0.025(2) Uani 1 1 d .
H3 H -0.2139 0.1135 0.6828 0.030 Uiso 1 1 calc R
C4 C -0.0933(8) 0.0481(5) 0.7274(8) 0.026(2) Uani 1 1 d .
H4 H -0.1364 0.0109 0.7384 0.031 Uiso 1 1 calc R
C5 C 0.0935(9) -0.0016(5) 0.7702(8) 0.027(2) Uani 1 1 d .
H5A H 0.0615 -0.0249 0.8290 0.040 Uiso 1 1 calc R
H5B H 0.1691 0.0137 0.7923 0.040 Uiso 1 1 calc R
H5C H 0.0986 -0.0299 0.7089 0.040 Uiso 1 1 calc R
C6 C 0.1165(8) 0.0689(4) 0.4820(8) 0.0230(19) Uani 1 1 d .
C7 C 0.2935(9) -0.0104(4) 0.5870(7) 0.024(2) Uani 1 1 d .
C8 C 0.4510(10) 0.0916(5) 0.5696(8) 0.029(2) Uani 1 1 d .
C9 C 0.2791(8) 0.1644(4) 0.4424(7) 0.0192(17) Uani 1 1 d .
C10 C 0.3269(8) 0.0446(4) 0.3867(8) 0.0232(19) Uani 1 1 d .
C11 C 0.4309(9) 0.1425(4) 0.8266(9) 0.029(2) Uani 1 1 d .
C12 C 0.5174(8) 0.1859(5) 0.8242(8) 0.027(2) Uani 1 1 d .
H12 H 0.5094 0.2302 0.8122 0.032 Uiso 1 1 calc R
C13 C 0.6207(9) 0.1527(5) 0.8428(8) 0.029(2) Uani 1 1 d .
H13 H 0.6944 0.1705 0.8464 0.035 Uiso 1 1 calc R
C14 C 0.5932(8) 0.0906(5) 0.8545(8) 0.025(2) Uani 1 1 d .
H14 H 0.6461 0.0573 0.8672 0.030 Uiso 1 1 calc R
C15 C 0.4237(9) 0.0222(5) 0.8534(9) 0.029(2) Uani 1 1 d .
H15A H 0.4786 -0.0120 0.8450 0.043 Uiso 1 1 calc R
H15B H 0.3636 0.0189 0.7975 0.043 Uiso 1 1 calc R
H15C H 0.3911 0.0185 0.9231 0.043 Uiso 1 1 calc R
C16 C 0.1891(9) 0.0434(5) 1.0184(7) 0.027(2) Uani 1 1 d .
C17 C 0.0275(10) 0.1405(4) 0.9676(8) 0.029(2) Uani 1 1 d .
C18 C 0.1941(8) 0.2361(4) 1.0479(7) 0.0214(18) Uani 1 1 d .
C19 C 0.3564(9) 0.1368(5) 1.0831(9) 0.029(2) Uani 1 1 d .
C20 C 0.1369(9) 0.1333(5) 1.1668(7) 0.024(2) Uani 1 1 d .
C21 C 0.0869(8) 0.2692(5) 0.8084(7) 0.0217(19) Uani 1 1 d .
C22 C 0.1250(8) 0.2419(4) 0.5881(7) 0.0219(19) Uani 1 1 d .
C23 C 0.3705(8) 0.2458(4) 0.6369(7) 0.0199(18) Uani 1 1 d .
C24 C 0.3226(8) 0.2935(4) 0.8477(7) 0.0216(18) Uani 1 1 d .
C25 C 0.2200(8) 0.3459(4) 0.6714(7) 0.0187(17) Uani 1 1 d .
N1 N 0.0219(7) 0.0518(4) 0.7414(6) 0.0202(16) Uani 1 1 d .
N2 N 0.4794(7) 0.0829(4) 0.8456(6) 0.0222(16) Uani 1 1 d .
O1 O 0.0223(7) 0.0633(3) 0.4579(6) 0.0330(17) Uani 1 1 d .
O2 O 0.3025(7) -0.0614(3) 0.6135(6) 0.0375(18) Uani 1 1 d .
O3 O 0.5450(7) 0.0962(4) 0.5908(7) 0.0361(18) Uani 1 1 d .
O4 O 0.2758(6) 0.2074(3) 0.3897(6) 0.0273(15) Uani 1 1 d .
O5 O 0.3497(6) 0.0274(4) 0.3054(5) 0.0310(16) Uani 1 1 d .
O6 O 0.1842(7) -0.0108(3) 1.0225(6) 0.0356(18) Uani 1 1 d .
O7 O -0.0674(7) 0.1405(4) 0.9472(7) 0.042(2) Uani 1 1 d .
O8 O 0.1959(6) 0.2882(3) 1.0698(6) 0.0335(17) Uani 1 1 d .
O9 O 0.4483(8) 0.1344(4) 1.1185(8) 0.050(2) Uani 1 1 d .
O10 O 0.0989(8) 0.1308(4) 1.2485(6) 0.040(2) Uani 1 1 d .
O11 O 0.0111(7) 0.2812(4) 0.8550(6) 0.0385(19) Uani 1 1 d .
O12 O 0.0665(7) 0.2369(4) 0.5146(6) 0.0350(17) Uani 1 1 d .
O13 O 0.4480(6) 0.2433(3) 0.5899(6) 0.0304(16) Uani 1 1 d .
O14 O 0.3711(6) 0.3202(4) 0.9130(6) 0.0361(18) Uani 1 1 d .
O15 O 0.2172(7) 0.3967(3) 0.6422(6) 0.0300(16) Uani 1 1 d .
P1 P 0.2014(2) 0.13189(11) 0.68876(19) 0.0227(5) Uani 1 1 d .
P2 P 0.2798(2) 0.15613(12) 0.8414(2) 0.0232(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'
N N 0.0061 0.0033 '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
C10 W1 C6 90.3(4)
C10 W1 C8 89.5(4)
C6 W1 C8 179.7(4)
C10 W1 C9 82.8(4)
C6 W1 C9 87.8(4)
C8 W1 C9 92.2(4)
C10 W1 C7 88.0(4)
C6 W1 C7 91.6(4)
C8 W1 C7 88.3(4)
C9 W1 C7 170.8(4)
C10 W1 P1 171.4(3)
C6 W1 P1 82.2(3)
C8 W1 P1 98.0(3)
C9 W1 P1 92.6(3)
C7 W1 P1 96.4(3)
C20 W2 C16 86.6(4)
C20 W2 C19 90.4(4)
C16 W2 C19 90.1(4)
C20 W2 C17 86.8(4)
C16 W2 C17 88.7(4)
C19 W2 C17 177.0(4)
C20 W2 C18 85.4(4)
C16 W2 C18 171.9(4)
C19 W2 C18 88.5(4)
C17 W2 C18 92.3(4)
C20 W2 P2 174.6(3)
C16 W2 P2 97.3(3)
C19 W2 P2 85.8(3)
C17 W2 P2 97.0(3)
C18 W2 P2 90.6(3)
C22 W3 C25 81.0(4)
C22 W3 C23 92.0(4)
C25 W3 C23 86.6(3)
C22 W3 C21 89.5(4)
C25 W3 C21 89.4(4)
C23 W3 C21 175.4(4)
C22 W3 C24 163.2(4)
C25 W3 C24 82.4(4)
C23 W3 C24 90.0(4)
C21 W3 C24 87.3(4)
C22 W3 P2 119.7(3)
C25 W3 P2 159.2(3)
C23 W3 P2 93.4(3)
C21 W3 P2 89.6(3)
C24 W3 P2 76.8(3)
C22 W3 P1 71.9(3)
C25 W3 P1 151.6(3)
C23 W3 P1 86.2(2)
C21 W3 P1 98.4(3)
C24 W3 P1 125.0(3)
P2 W3 P1 48.79(8)
N1 C1 C2 105.0(8)
N1 C1 P1 121.9(7)
C2 C1 P1 130.6(8)
C3 C2 C1 109.0(9)
C3 C2 H2 125.5
C1 C2 H2 125.5
C4 C3 C2 106.8(9)
C4 C3 H3 126.6
C2 C3 H3 126.6
C3 C4 N1 110.7(9)
C3 C4 H4 124.7
N1 C4 H4 124.7
N1 C5 H5A 109.5
N1 C5 H5B 109.5
H5A C5 H5B 109.5
N1 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
O1 C6 W1 179.1(9)
O2 C7 W1 174.8(8)
O3 C8 W1 177.4(9)
O4 C9 W1 174.6(8)
O5 C10 W1 176.3(8)
C12 C11 N2 107.4(9)
C12 C11 P2 129.3(7)
N2 C11 P2 121.3(7)
C11 C12 C13 108.0(9)
C11 C12 H12 126.0
C13 C12 H12 126.0
C14 C13 C12 106.4(9)
C14 C13 H13 126.8
C12 C13 H13 126.8
C13 C14 N2 110.4(8)
C13 C14 H14 124.8
N2 C14 H14 124.8
N2 C15 H15A 109.5
N2 C15 H15B 109.5
H15A C15 H15B 109.5
N2 C15 H15C 109.5
H15A C15 H15C 109.5
H15B C15 H15C 109.5
O6 C16 W2 175.8(8)
O7 C17 W2 173.5(9)
O8 C18 W2 175.1(9)
O9 C19 W2 179.1(10)
O10 C20 W2 176.4(9)
O11 C21 W3 176.2(9)
O12 C22 W3 178.1(9)
O13 C23 W3 178.0(8)
O14 C24 W3 173.9(9)
O15 C25 W3 178.7(9)
C4 N1 C1 108.5(8)
C4 N1 C5 123.9(8)
C1 N1 C5 127.4(8)
C14 N2 C11 107.8(8)
C14 N2 C15 123.8(8)
C11 N2 C15 128.4(8)
C1 P1 P2 104.9(4)
C1 P1 W1 117.4(3)
P2 P1 W1 130.63(14)
C1 P1 W3 106.9(3)
P2 P1 W3 65.37(9)
W1 P1 W3 119.78(10)
C11 P2 P1 104.7(4)
C11 P2 W2 120.3(4)
P1 P2 W2 125.88(13)
C11 P2 W3 105.7(3)
P1 P2 W3 65.84(9)
W2 P2 W3 121.74(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 C10 2.002(9)
W1 C6 2.046(10)
W1 C8 2.048(12)
W1 C9 2.059(9)
W1 C7 2.061(9)
W1 P1 2.556(2)
W2 C20 1.982(9)
W2 C16 2.031(10)
W2 C19 2.045(11)
W2 C17 2.054(12)
W2 C18 2.056(9)
W2 P2 2.564(3)
W3 C22 2.043(10)
W3 C25 2.044(9)
W3 C23 2.055(9)
W3 C21 2.067(10)
W3 C24 2.077(9)
W3 P2 2.605(2)
W3 P1 2.615(2)
C1 N1 1.395(12)
C1 C2 1.404(14)
C1 P1 1.823(11)
C2 C3 1.402(14)
C2 H2 0.9500
C3 C4 1.331(14)
C3 H3 0.9500
C4 N1 1.371(12)
C4 H4 0.9500
C5 N1 1.445(12)
C5 H5A 0.9800
C5 H5B 0.9800
C5 H5C 0.9800
C6 O1 1.149(12)
C7 O2 1.129(12)
C8 O3 1.137(13)
C9 O4 1.124(11)
C10 O5 1.132(11)
C11 C12 1.375(14)
C11 N2 1.397(12)
C11 P2 1.834(11)
C12 C13 1.419(14)
C12 H12 0.9500
C13 C14 1.358(14)
C13 H13 0.9500
C14 N2 1.359(12)
C14 H14 0.9500
C15 N2 1.444(12)
C15 H15A 0.9800
C15 H15B 0.9800
C15 H15C 0.9800
C16 O6 1.145(12)
C17 O7 1.142(14)
C18 O8 1.132(12)
C19 O9 1.159(13)
C20 O10 1.146(12)
C21 O11 1.126(12)
C22 O12 1.135(12)
C23 O13 1.119(12)
C24 O14 1.131(12)
C25 O15 1.131(11)
P1 P2 2.156(4)
