#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:07:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178491 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/02/4060269.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_4060269
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om0343061
_journal_year                    2004
_chemical_formula_sum            'C40 H30 O4 P2 W'
_chemical_formula_weight         820.43
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.5948(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4288(4)
_cell_length_b                   16.9288(7)
_cell_length_c                   21.2946(9)
_cell_measurement_reflns_used    6572
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.03
_cell_measurement_theta_min      2.22
_cell_volume                     3329.6(2)
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'BRUKER SMART APEX 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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33047
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    3.607
_exptl_absorpt_correction_T_max  0.7863
_exptl_absorpt_correction_T_min  0.5791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0365
_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)+(0.0452P)²+0.5971P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0912
_reflns_number_gt                6471
_reflns_number_total             7644
_reflns_threshold_expression     >2sigma(I)
_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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4060269
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
_atom_site_disorder_assembly
_atom_site_disorder_group
W W 0.772100(17) 0.726539(10) 0.196041(8) 0.03243(7) Uani 1 1 d . . .
P1 P 0.88584(12) 0.68560(6) 0.31225(5) 0.0328(2) Uani 1 1 d . . .
P2 P 0.97011(11) 0.68004(7) 0.13820(5) 0.0329(2) Uani 1 1 d . . .
O1 O 0.4833(4) 0.7665(2) 0.2402(2) 0.0682(11) Uani 1 1 d . . .
O2 O 0.6297(5) 0.8166(2) 0.0705(2) 0.0782(13) Uani 1 1 d . . .
O3 O 0.9157(3) 0.81663(17) 0.22863(14) 0.0407(7) Uani 1 1 d . . .
O4 O 0.7097(3) 0.61004(17) 0.18010(14) 0.0384(7) Uani 1 1 d . . .
C1 C 0.5877(5) 0.7491(3) 0.2249(2) 0.0426(11) Uani 1 1 d . . .
C2 C 0.6879(6) 0.7862(3) 0.1165(3) 0.0473(12) Uani 1 1 d . . .
C3 C 0.7974(5) 0.8399(3) 0.2493(2) 0.0416(10) Uani 1 1 d . . .
H3A H 0.7463 0.8847 0.2257 0.050 Uiso 1 1 calc R . .
C4 C 0.7956(5) 0.8388(3) 0.3186(2) 0.0394(10) Uani 1 1 d . . .
C5 C 0.7511(5) 0.9049(3) 0.3482(3) 0.0512(12) Uani 1 1 d . . .
H5A H 0.7301 0.9515 0.3251 0.061 Uiso 1 1 calc R . .
C6 C 0.7378(6) 0.9023(3) 0.4113(3) 0.0563(14) Uani 1 1 d . . .
H6A H 0.7048 0.9465 0.4300 0.068 Uiso 1 1 calc R . .
C7 C 0.7727(6) 0.8355(3) 0.4466(3) 0.0571(14) Uani 1 1 d . . .
H7A H 0.7623 0.8342 0.4891 0.068 Uiso 1 1 calc R . .
C8 C 0.8242(6) 0.7689(3) 0.4195(2) 0.0470(12) Uani 1 1 d . . .
H8A H 0.8520 0.7240 0.4441 0.056 Uiso 1 1 calc R . .
C9 C 0.8330(5) 0.7705(2) 0.3553(2) 0.0377(10) Uani 1 1 d . . .
C10 C 0.8205(5) 0.6001(2) 0.3503(2) 0.0359(9) Uani 1 1 d . . .
C11 C 0.8869(6) 0.5724(3) 0.4104(2) 0.0523(13) Uani 1 1 d . . .
H11A H 0.9724 0.5957 0.4319 0.063 Uiso 1 1 calc R . .
C12 C 0.8271(7) 0.5107(3) 0.4384(3) 0.0644(15) Uani 1 1 d . . .
H12A H 0.8726 0.4921 0.4785 0.077 Uiso 1 1 calc R . .
C13 C 0.7002(6) 0.4769(3) 0.4070(3) 0.0626(15) Uani 1 1 d . . .
H13A H 0.6590 0.4361 0.4265 0.075 Uiso 1 1 calc R . .
C14 C 0.6339(5) 0.5025(3) 0.3475(3) 0.0520(13) Uani 1 1 d . . .
H14A H 0.5489 0.4786 0.3262 0.062 Uiso 1 1 calc R . .
C15 C 0.6939(5) 0.5642(3) 0.3193(2) 0.0435(11) Uani 1 1 d . . .
H15A H 0.6486 0.5819 0.2789 0.052 Uiso 1 1 calc R . .
C16 C 1.0819(5) 0.6823(3) 0.3374(2) 0.0376(10) Uani 1 1 d . . .
C17 C 1.1568(5) 0.6113(3) 0.3385(2) 0.0498(12) Uani 1 1 d . . .
H17A H 1.1055 0.5643 0.3297 0.060 Uiso 1 1 calc R . .
C18 C 1.3052(6) 0.6096(4) 0.3524(3) 0.0622(15) Uani 1 1 d . . .
H18A H 1.3536 0.5616 0.3539 0.075 Uiso 1 1 calc R . .
C19 C 1.3823(6) 0.6784(4) 0.3643(3) 0.0623(15) Uani 1 1 d . . .
H19A H 1.4830 0.6773 0.3729 0.075 Uiso 1 1 calc R . .
C20 C 1.3106(6) 0.7487(4) 0.3634(3) 0.0620(15) Uani 1 1 d . . .
H20A H 1.3630 0.7954 0.3719 0.074 Uiso 1 1 calc R . .
C21 C 1.1617(6) 0.7512(3) 0.3499(3) 0.0508(12) Uani 1 1 d . . .
H21A H 1.1143 0.7994 0.3493 0.061 Uiso 1 1 calc R . .
C22 C 0.6533(5) 0.6450(3) 0.1232(2) 0.0381(10) Uani 1 1 d . . .
H22A H 0.5478 0.6512 0.1140 0.046 Uiso 1 1 calc R . .
C23 C 0.7174(5) 0.6230(3) 0.0668(2) 0.0372(10) Uani 1 1 d . . .
C24 C 0.6292(5) 0.5905(3) 0.0121(2) 0.0466(11) Uani 1 1 d . . .
H24A H 0.5299 0.5867 0.0098 0.056 Uiso 1 1 calc R . .
C25 C 0.6872(6) 0.5644(3) -0.0379(2) 0.0522(13) Uani 1 1 d . . .
H25A H 0.6272 0.5435 -0.0741 0.063 Uiso 1 1 calc R . .
C26 C 0.8328(6) 0.5689(3) -0.0348(2) 0.0495(12) Uani 1 1 d . . .
H26A H 0.8720 0.5499 -0.0686 0.059 Uiso 1 1 calc R . .
C27 C 0.9226(5) 0.6016(3) 0.0183(2) 0.0417(10) Uani 1 1 d . . .
H27A H 1.0220 0.6041 0.0203 0.050 Uiso 1 1 calc R . .
C28 C 0.8647(5) 0.6307(3) 0.0682(2) 0.0364(9) Uani 1 1 d . . .
C29 C 1.0634(5) 0.7616(3) 0.1089(2) 0.0368(10) Uani 1 1 d . . .
C30 C 1.0317(6) 0.7889(3) 0.0462(2) 0.0518(13) Uani 1 1 d . . .
H30A H 0.9629 0.7626 0.0159 0.062 Uiso 1 1 calc R . .
C31 C 1.1010(7) 0.8545(3) 0.0279(3) 0.0706(17) Uani 1 1 d . . .
H31A H 1.0788 0.8719 -0.0144 0.085 Uiso 1 1 calc R . .
C32 C 1.2016(7) 0.8937(4) 0.0717(3) 0.0714(18) Uani 1 1 d . . .
H32A H 1.2485 0.9378 0.0596 0.086 Uiso 1 1 calc R . .
C33 C 1.2329(7) 0.8676(3) 0.1339(3) 0.0668(16) Uani 1 1 d . . .
H33A H 1.3018 0.8943 0.1638 0.080 Uiso 1 1 calc R . .
C34 C 1.1649(6) 0.8029(3) 0.1529(2) 0.0489(12) Uani 1 1 d . . .
H34A H 1.1869 0.7867 0.1955 0.059 Uiso 1 1 calc R . .
C35 C 1.1082(5) 0.6051(3) 0.1673(2) 0.0360(9) Uani 1 1 d . . .
C36 C 1.2538(5) 0.6119(3) 0.1662(2) 0.0430(11) Uani 1 1 d . . .
H36A H 1.2895 0.6582 0.1517 0.052 Uiso 1 1 calc R . .
C37 C 1.3466(5) 0.5490(3) 0.1869(2) 0.0497(12) Uani 1 1 d . . .
H37A H 1.4447 0.5538 0.1868 0.060 Uiso 1 1 calc R . .
C38 C 1.2948(6) 0.4800(3) 0.2076(2) 0.0552(14) Uani 1 1 d . . .
H38A H 1.3575 0.4381 0.2210 0.066 Uiso 1 1 calc R . .
C39 C 1.1500(6) 0.4730(3) 0.2082(2) 0.0522(13) Uani 1 1 d . . .
H39A H 1.1142 0.4260 0.2213 0.063 Uiso 1 1 calc R . .
C40 C 1.0580(5) 0.5351(3) 0.1895(2) 0.0435(11) Uani 1 1 d . . .
H40A H 0.9608 0.5305 0.1916 0.052 Uiso 1 1 calc R . .
