#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:44:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178791 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/45/4104512.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_4104512
loop_
_publ_author_name
'Matthew P. Duffy'
'François Mathey'
_publ_section_title
;
 Generation and Trapping of a Terminal Chlorophosphinidene Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7534
_journal_page_last               7535
_journal_paper_doi               10.1021/ja901918e
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C11 H8 Cl O5 P W'
_chemical_formula_sum            'C11 H8 Cl O5 P W'
_chemical_formula_weight         470.44
_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                107.800(7)
_cell_angle_beta                 95.428(7)
_cell_angle_gamma                107.102(5)
_cell_formula_units_Z            2
_cell_length_a                   6.6527(7)
_cell_length_b                   10.8920(11)
_cell_length_c                   11.9177(19)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      2.24
_cell_volume                     769.56(17)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17156
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    7.792
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.1466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         4047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0167
_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)+(0.0174P)²+0.3615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                3684
_reflns_number_total             4047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901918e_si_001.cif
_cod_data_source_block           mat5t
_cod_original_cell_volume        769.55(17)
_cod_database_code               4104512
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
W1 W 0.116678(16) 0.849200(10) 0.676313(9) 0.04229(4) Uani 1 1 d .
C1 C -0.2121(5) 0.5421(3) 0.7356(3) 0.0594(7) Uani 1 1 d .
H1 H -0.3484 0.5199 0.6909 0.071 Uiso 1 1 calc R
C2 C -0.1347(6) 0.4522(3) 0.7616(3) 0.0630(8) Uani 1 1 d .
C3 C 0.0831(6) 0.5146(4) 0.8377(3) 0.0690(9) Uani 1 1 d .
C4 C 0.1592(6) 0.6506(4) 0.8704(3) 0.0734(10) Uani 1 1 d .
H4 H 0.2880 0.7071 0.9239 0.088 Uiso 1 1 calc R
C5 C -0.2528(10) 0.3008(4) 0.7188(5) 0.1152(19) Uani 1 1 d .
H5A H -0.3020 0.2758 0.7846 0.173 Uiso 1 1 calc R
H5B H -0.1584 0.2526 0.6886 0.173 Uiso 1 1 calc R
H5C H -0.3738 0.2769 0.6558 0.173 Uiso 1 1 calc R
C6 C 0.2005(10) 0.4285(7) 0.8724(5) 0.123(2) Uani 1 1 d .
H6A H 0.3357 0.4872 0.9251 0.184 Uiso 1 1 calc R
H6B H 0.2252 0.3685 0.8013 0.184 Uiso 1 1 calc R
H6C H 0.1156 0.3749 0.9128 0.184 Uiso 1 1 calc R
C7 C 0.3399(5) 0.9894(3) 0.8233(3) 0.0587(7) Uani 1 1 d .
C8 C -0.0941(5) 0.9512(3) 0.7220(3) 0.0583(7) Uani 1 1 d .
C9 C 0.2300(5) 0.9684(3) 0.5812(3) 0.0572(7) Uani 1 1 d .
C10 C -0.1044(5) 0.7111(4) 0.5262(3) 0.0587(7) Uani 1 1 d .
C11 C 0.3244(5) 0.7456(3) 0.6329(3) 0.0580(7) Uani 1 1 d .
Cl1 Cl -0.1529(3) 0.80211(13) 0.93369(13) 0.1187(5) Uani 1 1 d .
O1 O 0.4637(5) 1.0694(3) 0.9035(3) 0.0984(10) Uani 1 1 d .
O2 O -0.2062(5) 1.0099(3) 0.7479(3) 0.0893(9) Uani 1 1 d .
O3 O 0.2917(5) 1.0389(3) 0.5291(3) 0.0899(9) Uani 1 1 d .
O4 O -0.2234(5) 0.6353(3) 0.4416(3) 0.0928(9) Uani 1 1 d .
O5 O 0.4413(5) 0.6884(3) 0.6081(3) 0.0955(10) Uani 1 1 d .
P1 P -0.01979(13) 0.70967(7) 0.79775(7) 0.05005(16) 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'
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'
Cl Cl 0.1484 0.1585 '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
C9 W1 C7 88.88(13)
C9 W1 C11 91.62(14)
C7 W1 C11 90.21(14)
C9 W1 C10 89.73(13)
C7 W1 C10 178.61(13)
C11 W1 C10 89.72(14)
C9 W1 C8 89.48(13)
C7 W1 C8 89.73(14)
C11 W1 C8 178.90(13)
C10 W1 C8 90.37(14)
C9 W1 P1 178.30(9)
C7 W1 P1 89.75(10)
C11 W1 P1 89.39(10)
C10 W1 P1 91.64(10)
C8 W1 P1 89.51(10)
C2 C1 P1 110.6(3)
C1 C2 C3 113.9(3)
C1 C2 C5 124.4(4)
C3 C2 C5 121.7(4)
C4 C3 C2 113.2(3)
C4 C3 C6 125.3(4)
C2 C3 C6 121.6(4)
C3 C4 P1 110.6(3)
O1 C7 W1 178.4(4)
O2 C8 W1 178.5(3)
O3 C9 W1 178.0(3)
O4 C10 W1 178.4(3)
O5 C11 W1 179.4(3)
C1 P1 C4 91.24(17)
C1 P1 Cl1 101.66(13)
C4 P1 Cl1 103.85(15)
C1 P1 W1 123.22(12)
C4 P1 W1 118.84(13)
Cl1 P1 W1 114.13(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 C9 2.006(3)
W1 C7 2.036(3)
W1 C11 2.036(3)
W1 C10 2.045(3)
W1 C8 2.047(3)
W1 P1 2.4516(8)
C1 C2 1.331(5)
C1 P1 1.772(3)
C2 C3 1.476(5)
C2 C5 1.499(5)
C3 C4 1.332(5)
C3 C6 1.506(5)
C4 P1 1.783(4)
C7 O1 1.127(4)
C8 O2 1.124(4)
C9 O3 1.139(4)
C10 O4 1.132(4)
C11 O5 1.139(4)
Cl1 P1 2.0546(13)
