#------------------------------------------------------------------------------
#$Date: 2022-09-28 18:08:17 +0300 (Wed, 28 Sep 2022) $
#$Revision: 278247 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/96/2009624.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2009624
loop_
_publ_author_name
'Du, S.'
'Wu, X.'
_publ_section_title
;μ-(O,O'-Diethyl
 dithiophosphato-2κS:3κS')-oxo-1κO-tri-μ₃-sulfido-1:2:3κ³S;1:2:4κ³S;1:3:4κ³S-tris(triphenylphosphine)-2κP;3κP;4κP-tricoppertungsten
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              500
_journal_page_last               502
_journal_paper_doi               10.1107/S0108270193009023
_journal_volume                  50
_journal_year                    1994
_chemical_formula_sum            'C58 H55 Cu3 O3 P4 S5 W'
_chemical_formula_weight         1458.75
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source           'Cromer & Waber (1974)'
_cell_angle_alpha                99.27(3)
_cell_angle_beta                 107.08(3)
_cell_angle_gamma                88.12(3)
_cell_formula_units_Z            2
_cell_length_a                   13.808(6)
_cell_length_b                   19.764(6)
_cell_length_c                   11.696(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      6
_cell_volume                     3011(2)
_diffrn_measurement_device       'Rigaku AFC-5R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.02703
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11084
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.306
_exptl_absorpt_correction_T_max  1.0417
_exptl_absorpt_correction_T_min  0.9559
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.61
_exptl_crystal_description       cubic
_exptl_crystal_size_min          'not measured'
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.81
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.58
_refine_ls_number_parameters     377
_refine_ls_number_reflns         8310
_refine_ls_R_factor_obs          0.045
_refine_ls_shift/esd_max         0.37
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/σ²(Fₒ)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.063
_reflns_number_observed          8310
_reflns_number_total             10598
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            hu1053.cif
_cod_data_source_block           hu1053_structure_1_of_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/\s^2^(F~o~)' 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^(F~o~)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C58 H55 Cu3 O3 P4 S5 W1'
_cod_database_code               2009624
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
W -.19315(2) .18398(2) .20611(3)
Cu(1) -.29787(7) .21002(5) -.02422(8)
Cu(2) -.23510(8) .32250(5) .21520(10)
Cu(3) -.02204(7) .22964(5) .16106(9)
S(1) -.34950(10) .22770(10) .1547(2)
S(2) -.14710(10) .15130(10) .0360(2)
S(3) -.08930(10) .27040(10) .3201(2)
S(4) -.2534(2) .33150(10) -.0129(2)
S(5) .0048(2) .32760(10) .0853(3)
P(1) -.4272(2) .16490(10) -.1825(2)
P(2) -.2791(2) .42110(10) .3068(2)
P(3) .13100(10) .17560(10) .2053(2)
P(4) -.1203(2) .33300(10) -.0482(2)
O(1) -.1910(5) .1163(3) .2819(6)
O(2) -.1274(5) .2752(4) -.1610(6)
O(3) -.1113(7) .3979(5) -.1080(10)
C(1) -.039(2) .2390(10) -.187(2)
C(2) -.031(2) .2350(10) -.292(3)
C(3) -.131(2) .4580(10) -.072(2)
C(4) -.1500(10) .5082(9) -.1550(10)
C(111) -.4658(6) .0815(4) -.1632(7)
C(112) -.5666(6) .0593(4) -.1919(7)
C(113) -.5884(7) -.0067(5) -.1768(8)
C(114) -.5017(7) -.0503(5) -.1375(8)
C(115) -.4113(7) -.0292(5) -.1078(8)
C(116) -.3886(6) .0357(4) -.1209(7)
C(121) -.5423(7) .2164(5) -.2061(8)
C(122) -.5770(8) .2395(5) -.1080(10)
C(123) -.6640(10) .2797(7) -.1200(10)
C(124) -.7120(10) .2961(7) -.2310(10)
C(125) -.6820(10) .2758(9) -.3260(10)
C(126) -.5920(10) .2357(7) -.3170(10)
C(131) -.4068(6) .1472(4) -.3311(7)
C(132) -.4717(7) .1051(5) -.4292(8)
C(133) -.4517(7) .0933(5) -.5411(9)
C(134) -.3717(7) .1227(5) -.5554(9)
C(135) -.3032(9) .1621(6) -.4590(10)
C(136) -.3217(7) .1742(5) -.3473(9)
C(211) -.3089(6) .4107(4) .4449(7)
C(212) -.3667(6) .4581(5) .4973(8)
C(213) -.3919(7) .4470(5) .5994(8)
C(214) -.3589(9) .3899(6) .6500(10)
C(215) -.3010(10) .3439(8) .6000(10)
C(216) -.2759(8) .3537(6) .4980(10)
C(221) -.3938(6) .4607(4) .2230(7)
C(222) -.3998(7) .5311(5) .2182(8)
C(223) -.4919(8) .5576(5) .1537(9)
C(224) -.5719(7) .5176(5) .0996(9)
C(225) -.5679(8) .4483(6) .1030(10)
C(226) -.4774(7) .4187(5) .1643(8)
C(231) -.1838(6) .4895(5) .3527(8)
C(232) -.1400(10) .5030(6) .2660(10)
C(233) -.0670(10) .5572(7) .2940(10)
C(234) -.0390(10) .5929(7) .4090(10)
C(235) -.0780(10) .5792(7) .4930(10)
C(236) -.1512(8) .5269(6) .4670(10)
C(311) .2438(6) .2315(5) .2692(7)
C(312) .3403(9) .2087(6) .2760(10)
C(313) .4250(10) .2521(7) .3270(10)
C(314) .4120(10) .3179(8) .3680(10)
C(315) .3150(10) .3420(9) .3600(10)
C(316) .2310(10) .2972(7) .3110(10)
C(321) .1488(6) .1287(4) .0649(7)
C(322) .1099(7) .0628(5) .0205(9)
C(323) .1109(8) .0303(6) -.0940(10)
C(324) .1509(8) .0625(5) -.1640(10)
C(325) .1911(8) .1281(5) -.1207(9)
C(326) .1892(7) .1609(5) -.0059(8)
C(331) .1500(6) .1122(4) .3072(7)
C(332) .0913(9) .1159(6) .3840(10)
C(333) .1010(10) .0683(8) .4660(10)
C(334) .1730(10) .0201(8) .4690(10)
C(335) .2330(10) .0157(7) .3940(10)
C(336) .2200(10) .0619(6) .3110(10)
H1 .0197 .2611 -.1317
H2 -.0429 .1931 -.1721
H3 .0274 .2088 -.2965
H4 -.0892 .2136 -.3489
H5 -.0227 .2799 -.3070
H6 -.1890 .4563 -.0452
H7 -.0745 .4750 -.0051
H8 -.1626 .5515 -.1127
H9 -.0933 .5116 -.1828
H10 -.2082 .4939 -.2209
H11 -.6203 .0891 -.2215
H12 -.6568 -.0214 -.1939
H13 -.5259 -.0957 -.1307
H14 -.3583 -.0596 -.0782
H15 -.3197 .0498 -.1011
H16 -.5415 .2280 -.0313
H17 -.6883 .2952 -.0526
H18 -.7709 .3237 -.2399
H19 -.7195 .2876 -.4022
H20 -.5675 .2227 -.3853
H21 -.5295 .0843 -.4198
H22 -.4958 .0643 -.6075
H23 -.3614 .1164 -.6334
H24 -.2442 .1807 -.4697
H25 -.2751 .2015 -.2808
H26 -.3891 .4984 .4629
H27 -.4322 .4792 .6338
H28 -.3759 .3823 .7204
H29 -.2781 .3043 .6365
H30 -.2358 .3209 .4639
H31 -.3425 .5605 .2578
H32 -.4965 .6053 .1493
H33 -.6335 .5369 .0578
H34 -.6265 .4203 .0629
H35 -.4740 .3706 .1655
H36 -.1584 .4760 .1872
H37 -.0393 .5684 .2344
H38 -.0112 .6268 .4292
H39 -.0569 .6051 .5719
H40 -.1782 .5174 .5292
H41 .3496 .1622 .2450
H42 .4907 .2351 .3325
H43 .4688 .3481 .4018
H44 .3061 .3892 .3875
H45 .1648 .3138 .3083
H46 .0821 .0394 .0688
H47 .0832 -.0148 -.1233
H48 .1515 .0401 -.2419
H49 .2198 .1509 -.1690
H50 .2165 .2060 .0231
H51 .0427 .1513 .3826
H52 .0580 .0703 .5174
H53 .1819 -.0116 .5245
H54 .2830 -.0185 .3983
H55 .2609 .0578 .2573
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cu(2) W Cu(1) 70.38(5) yes
Cu(2) W Cu(3) 80.31(4) yes
Cu(3) W Cu(1) 85.95(5) yes
S(1) W S(2) 108.48(8) yes
S(1) W S(3) 106.38(8) yes
S(3) W S(2) 107.97(8) yes
O(1) W S(1) 110.4(2) yes
O(1) W S(2) 111.1(2) yes
O(1) W S(3) 112.3(2) yes
S(1) Cu(1) S(4) 95.28(9) yes
S(2) Cu(1) S(1) 101.94(8) yes
S(2) Cu(1) S(4) 107.51(8) yes
S(3) Cu(2) S(1) 99.89(9) yes
S(3) Cu(3) S(2) 102.32(8) yes
S(3) Cu(3) S(5) 104.80(10) yes
S(5) Cu(3) S(2) 117.50(10) yes
P(1) Cu(1) S(1) 109.70(9) yes
P(1) Cu(1) S(2) 121.42(9) yes
P(1) Cu(1) S(4) 116.80(10) yes
P(2) Cu(2) S(1) 119.50(10) yes
P(2) Cu(2) S(3) 117.42(9) yes
P(3) Cu(3) S(3) 118.21(9) yes
P(3) Cu(3) S(5) 105.60(10) yes
P(3) Cu(3) S(2) 109.03(9) yes
Cu(1) S(2) Cu(3) 108.32(9) yes
Cu(2) S(1) Cu(1) 84.79(8) yes
C(321) P(3) Cu(3) 109.0(3) yes
C(331) P(3) Cu(3) 117.6(3) yes
Cu(2) S(3) Cu(3) 100.00(10) yes
W S(1) Cu(2) 73.7(7) yes
W S(1) Cu(1) 73.89(7) yes
W S(2) Cu(1) 74.63(7) yes
W S(2) Cu(3) 74.25(7) yes
W S(3) Cu(2) 74.42(7) yes
W S(3) Cu(3) 74.40(7) yes
P(4) S(4) Cu(1) 107.10(10) yes
P(4) S(5) Cu(3) 103.40(10) yes
O(2) P(4) S(5) 112.5(3) yes
O(2) P(4) S(4) 106.4(3) yes
O(3) P(4) O(2) 99.1(5) yes
O(3) P(4) S(5) 108.3(4) yes
O(3) P(4) S(4) 110.6(3) yes
S(5) P(4) S(4) 118.3(2) yes
C(1) O(2) P(4) 124.0(10) yes
C(3) O(3) P(4) 127.0(10) yes
C(2) C(1) O(2) 118(2) yes
O(3) C(3) C(4) 120(2) yes
C(111) P(1) Cu(1) 111.3(3) yes
C(131) P(1) Cu(1) 118.1(3) yes
C(121) P(1) Cu(1) 114.1(3) yes
C(231) P(2) Cu(2) 115.5(3) yes
C(211) P(2) Cu(2) 111.7(3) yes
C(221) P(2) Cu(2) 116.6(3) yes
C(311) P(3) Cu(3) 116.2(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
W S(1) 2.247(2) yes
W S(2) 2.255(2) yes
W S(3) 2.249(2) yes
W O(1) 1.715(6) yes
W Cu(1) 2.779(2) yes
W Cu(2) 2.7710(10) yes
W Cu(3) 2.775(2) yes
Cu(1) S(1) 2.373(2) yes
Cu(1) S(2) 2.329(2) yes
Cu(1) S(4) 2.472(3) yes
Cu(1) P(1) 2.246(2) yes
Cu(2) S(1) 2.371(3) yes
Cu(2) S(3) 2.332(3) yes
Cu(2) P(2) 2.225(2) yes
Cu(3) S(2) 2.341(3) yes
Cu(3) S(3) 2.336(2) yes
Cu(3) S(5) 2.337(3) yes
Cu(3) P(3) 2.293(2) yes
S(4) P(4) 2.001(3) yes
S(5) P(4) 1.973(4) yes
P(4) O(2) 1.582(8) yes
P(4) O(3) 1.580(7) yes
O(2) C(1) 1.48(2) yes
O(3) C(3) 1.24(2) yes
C(1) C(2) 1.26(3) yes
C(3) C(4) 1.46(2) yes
P(1) C(111) 1.817(8) yes
P(1) C(121) 1.834(9) yes
P(1) C(131) 1.819(8) yes
P(2) C(211) 1.823(8) yes
P(2) C(221) 1.826(8) yes
P(2) C(231) 1.820(9) yes
P(3) C(311) 1.835(9) yes
P(3) C(321) 1.830(8) yes
P(3) C(331) 1.827(9) yes
