#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/21/4322195.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_4322195
loop_
_publ_author_name
'Paulo Pérez-Lourido'
'Jaime Romero'
'José A. García-Vázquez'
'Antonio Sousa'
'Kevin P. Maresca'
'Jon Zubieta'
_publ_section_title
;
 Synthesis and Characterization of Zinc and Cadmium Compounds with
 Arenephosphinothiol Ligands. Crystal and Molecular Structures of
 [Cd2{2-(Ph2PO)C6H4S}4], [Zn{2-(Ph2P)-6-(Me3Si)C6H3S}2],
 [Cd{2-(Ph2PO)-6-(Me3Si)C6H3S}2(CH3OH)], and [Zn{PhPO(C6H4S-2)2}(bipy)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3709
_journal_page_last               3715
_journal_paper_doi               10.1021/ic981405b
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C42 H37 Cd N3 O2 P2 S2'
_chemical_formula_weight         854.10
_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
_cell_angle_alpha                106.622(1)
_cell_angle_beta                 109.693(1)
_cell_angle_gamma                107.137(1)
_cell_formula_units_Z            2
_cell_length_a                   13.5780(2)
_cell_length_b                   13.8505(2)
_cell_length_c                   13.9526(2)
_cell_measurement_reflns_used    '60 frames'
_cell_measurement_temperature    298(2)
_cell_volume                     2133.30(7)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'Siemens XCIF'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       'ω 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  0.0235
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13594
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.5963
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.449
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_hydrogen_treatment    idealized
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9556
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_obs          0.0483
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(?P)²+?P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1613
_refine_ls_wR_factor_obs         0.1460
_reflns_number_total             9560
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981405b_1.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(?P)^2^+?P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(?P)^2^+?P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2133.30(5)
_cod_original_formula_sum        'C42 H37 N3 O2 P2 S2 Cd'
_cod_database_code               4322195
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cd Cd 0.3362(1) 0.3905(1) 0.4130(1) 0.040(1) Uani 1 d . .
S S 0.2490(1) 0.2909(1) 0.2028(1) 0.052(1) Uani 1 d . .
S S 0.5634(1) 0.4003(1) 0.4663(1) 0.039(1) Uani 1 d . .
P P 0.0446(1) 0.2794(1) 0.2884(1) 0.037(1) Uani 1 d . .
P P 0.3893(1) 0.1859(1) 0.4802(1) 0.038(1) Uani 1 d . .
O1 O 0.1498(2) 0.3602(2) 0.4001(2) 0.041(1) Uani 1 d . .
O2 O 0.3272(2) 0.2599(2) 0.4765(3) 0.047(1) Uani 1 d . .
C11 C 0.1318(4) 0.3197(3) 0.1402(3) 0.044(1) Uani 1 d . .
C12 C 0.1233(5) 0.3455(4) 0.0477(4) 0.057(1) Uani 1 d . .
C13 C 0.0326(5) 0.3669(4) -0.0084(4) 0.065(1) Uani 1 d . .
C14 C -0.0514(5) 0.3657(4) 0.0257(4) 0.064(1) Uani 1 d . .
C15 C -0.0472(4) 0.3397(4) 0.1151(4) 0.053(1) Uani 1 d . .
C16 C 0.0425(3) 0.3143(3) 0.1725(3) 0.041(1) Uani 1 d . .
C21 C -0.0762(5) 0.3541(4) 0.3928(5) 0.068(1) Uani 1 d . .
C22 C -0.1777(6) 0.3516(5) 0.4012(6) 0.090(2) Uani 1 d . .
C23 C -0.2840(5) 0.2731(6) 0.3182(7) 0.086(2) Uani 1 d . .
C24 C -0.2942(4) 0.1936(6) 0.2248(6) 0.078(2) Uani 1 d . .
C25 C -0.1955(4) 0.1936(4) 0.2146(4) 0.060(1) Uani 1 d . .
C26 C -0.0857(3) 0.2759(3) 0.2986(4) 0.046(1) Uani 1 d . .
C31 C 0.0472(4) 0.1014(4) 0.3375(4) 0.049(1) Uani 1 d . .
C32 C 0.0213(4) -0.0107(4) 0.3130(4) 0.059(1) Uani 1 d . .
C33 C -0.0290(5) -0.0874(4) 0.2019(5) 0.069(1) Uani 1 d . .
C34 C -0.0516(5) -0.0544(4) 0.1153(5) 0.069(1) Uani 1 d . .
C35 C -0.0258(4) 0.0577(4) 0.1398(4) 0.055(1) Uani 1 d . .
C36 C 0.0229(3) 0.1360(3) 0.2509(3) 0.040(1) Uani 1 d . .
C41 C 0.6152(3) 0.3514(3) 0.5697(3) 0.038(1) Uani 1 d . .
C42 C 0.7340(3) 0.4028(3) 0.6442(4) 0.048(1) Uani 1 d . .
C43 C 0.7800(4) 0.3648(4) 0.7238(4) 0.058(1) Uani 1 d . .
C44 C 0.7093(4) 0.2747(4) 0.7300(4) 0.061(1) Uani 1 d . .
C45 C 0.5906(4) 0.2219(4) 0.6564(4) 0.051(1) Uani 1 d . .
C46 C 0.5430(3) 0.2599(3) 0.5771(3) 0.040(1) Uani 1 d . .
C51 C 0.2943(5) 0.1224(5) 0.6104(5) 0.069(1) Uani 1 d . .
C52 C 0.2344(6) 0.0457(6) 0.6409(6) 0.087(2) Uani 1 d . .
C53 C 0.2031(5) -0.0675(6) 0.5851(6) 0.083(2) Uani 1 d . .
C54 C 0.2314(5) -0.1044(5) 0.5016(6) 0.072(2) Uani 1 d . .
C55 C 0.2918(4) -0.0288(4) 0.4702(5) 0.057(1) Uani 1 d . .
C56 C 0.3224(3) 0.0847(3) 0.5241(4) 0.044(1) Uani 1 d . .
C61 C 0.2716(4) 0.0536(5) 0.2512(4) 0.063(1) Uani 1 d . .
C62 C 0.2559(6) -0.0239(6) 0.1513(5) 0.088(2) Uani 1 d . .
C63 C 0.3467(6) -0.0471(5) 0.1462(5) 0.077(2) Uani 1 d . .
C64 C 0.4531(5) 0.0041(4) 0.2410(4) 0.063(1) Uani 1 d . .
C65 C 0.4683(4) 0.0787(4) 0.3411(4) 0.052(1) Uani 1 d . .
C66 C 0.3778(3) 0.1041(3) 0.3472(3) 0.041(1) Uani 1 d . .
N91 N -0.5735(16) 0.1388(24) -0.0082(19) 0.141(11) Uani 1 d . .
C91 C -0.6071(38) 0.1928(37) 0.0258(35) 0.166(17) Uani 1 d . .
C92 C -0.6377(24) 0.2503(26) -0.0277(28) 0.328(48) Uani 1 d . .
N93 N 0.0748(27) 0.3859(32) 0.7227(29) 0.169(13) Uani 1 d . .
C93 C 0.1380(29) 0.3794(33) 0.7083(30) 0.130(12) Uani 1 d . .
C94 C 0.2144(27) 0.4105(27) 0.6786(20) 0.131(12) Uani 1 d . .
N95 N 0.5737(23) 0.4292(19) 0.8701(27) 0.177(16) Uani 1 d . .
C95 C 0.6305(35) 0.4280(27) 0.9382(34) 0.350(64) Uani 1 d . .
C96 C 0.6403(30) 0.3534(31) 0.9705(30) 0.169(17) Uani 1 d . .
H12A H 0.1799(5) 0.3481(4) 0.0239(4) 0.068 Uiso 1 cal R .
H13A H 0.0286(5) 0.3824(4) -0.0699(4) 0.078 Uiso 1 cal R .
H14A H -0.1108(5) 0.3823(4) -0.0111(4) 0.077 Uiso 1 cal R .
H15A H -0.1043(4) 0.3388(4) 0.1379(4) 0.063 Uiso 1 cal R .
H21A H -0.0035(5) 0.4080(4) 0.4503(5) 0.081 Uiso 1 cal R .
H22A H -0.1714(6) 0.4045(5) 0.4644(6) 0.108 Uiso 1 cal R .
H23A H -0.3502(5) 0.2729(6) 0.3244(7) 0.103 Uiso 1 cal R .
H24A H -0.3673(4) 0.1396(6) 0.1682(6) 0.093 Uiso 1 cal R .
H25A H -0.2027(4) 0.1390(4) 0.1520(4) 0.071 Uiso 1 cal R .
H31A H 0.0808(4) 0.1534(4) 0.4119(4) 0.059 Uiso 1 cal R .
H32A H 0.0376(4) -0.0336(4) 0.3707(4) 0.071 Uiso 1 cal R .
H33A H -0.0479(5) -0.1625(4) 0.1853(5) 0.082 Uiso 1 cal R .
H34A H -0.0838(5) -0.1067(4) 0.0411(5) 0.083 Uiso 1 cal R .
H35A H -0.0412(4) 0.0803(4) 0.0818(4) 0.066 Uiso 1 cal R .
H42A H 0.7833(3) 0.4632(3) 0.6408(4) 0.058 Uiso 1 cal R .
H43A H 0.8591(4) 0.4007(4) 0.7730(4) 0.069 Uiso 1 cal R .
H44A H 0.7403(4) 0.2493(4) 0.7825(4) 0.074 Uiso 1 cal R .
H45A H 0.5424(4) 0.1609(4) 0.6600(4) 0.061 Uiso 1 cal R .
H51A H 0.3152(5) 0.1982(5) 0.6475(5) 0.082 Uiso 1 cal R .
H52A H 0.2155(6) 0.0705(6) 0.6987(6) 0.104 Uiso 1 cal R .
H53A H 0.1624(5) -0.1183(6) 0.6050(6) 0.099 Uiso 1 cal R .
H54A H 0.2105(5) -0.1802(5) 0.4651(6) 0.087 Uiso 1 cal R .
H55A H 0.3115(4) -0.0545(4) 0.4134(5) 0.069 Uiso 1 cal R .
H61A H 0.2113(4) 0.0713(5) 0.2534(4) 0.076 Uiso 1 cal R .
H62A H 0.1839(6) -0.0601(6) 0.0879(5) 0.106 Uiso 1 cal R .
H63A H 0.3362(6) -0.0973(5) 0.0788(5) 0.092 Uiso 1 cal R .
H64A H 0.5142(5) -0.0115(4) 0.2375(4) 0.076 Uiso 1 cal R .
H65A H 0.5396(4) 0.1122(4) 0.4051(4) 0.062 Uiso 1 cal R .
H92A H -0.6057(24) 0.3270(26) 0.0249(28) 0.492 Uiso 1 cal R .
H92B H -0.7208(24) 0.2204(26) -0.0652(28) 0.492 Uiso 1 cal R .
H92C H -0.6091(24) 0.2461(26) -0.0823(28) 0.492 Uiso 1 cal R .
H94A H 0.2183(27) 0.3463(27) 0.6332(20) 0.197 Uiso 1 cal R .
H94B H 0.2882(27) 0.4578(27) 0.7441(20) 0.197 Uiso 1 cal R .
H94C H 0.1954(27) 0.4513(27) 0.6355(20) 0.197 Uiso 1 cal R .
H96A H 0.6826(30) 0.3865(31) 1.0512(30) 0.254 Uiso 1 cal R .
H96B H 0.6811(30) 0.3199(31) 0.9386(30) 0.254 Uiso 1 cal R .
H96C H 0.5645(30) 0.2972(31) 0.9462(30) 0.254 Uiso 1 cal R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 '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 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
O2 Cd Ol 86.68(9) . . ?
O2 Cd Sl 106.44(8) . . ?
O1 Cd Sl 90.63(7) . . ?
O2 Cd S2#l 125.75(8) . . ?
O1 Cd S2#l 97.31(6) . . ?
S1 Cd S2#l 127.47(4) . . ?
O2 Cd S2 79.67(7) . . ?
O1 Cd S2 165.56(7) . . ?
S1 Cd S2 97.72(3) . . ?
S2#1 Cd S2 86.97(3) . . ?
C11 S1 Cd 109.29(13) . . ?
C41 S2 Cd#l 100.64(12) . . ?
C41 S2 Cd 114.79(13) . . ?
C#l S2 Cd 93.03(3) . . ?
O1 Pl C16 114.1(2) . . ?
O1 Pl C36 113.0(2) . . ?
C16 Pl C36 109.5(2) . . ?
O1 Pl C26 109.7(2) . . ?
C16 Pl C26 107.0(2) . . ?
C36 Pl C26 102.8(2) . . ?
O2 P2 C66 115.5(2) . . ?
O2 P2 C46 114.1(2) . . ?
C66 P2 C46 105.9(2) . . ?
O2 P2 C56 107.5(2) . . ?
C66 P2 C56 105.2(2) . . ?
C46 P2 C56 108.1(2) . . ?
P1 O1 Cd 118.22(14) . . ?
P2 O2 Cd 132.1(2) . . ?
C12 C11 C16 117.5(4) . . ?
C12 C11 Sl 117.5(3) . . ?
C16 C11 S1 124.9(3) . . ?
C13 C12 C11 121.6(5) . . ?
C14 C13 C12 120.7(4) . . ?
C15 C14 C13 119.7(4) . . ?
C14 C15 C16 121.1(4) . . ?
C15 C16 C11 119.3(4) . . ?
C15 C16 P1 120.0(3) . . ?
C11 C16 P1 120.7(3) . . ?
C26 C21 C22 119.5(5) . . ?
C23 C22 C21 120.8(5) . . ?
C22 C23 C24 120.0(5) . . ?
C23 C24 C25 120.4(5) . . ?
C26 C25 C24 119.8(5) . . ?
C21 C26 C25 119.4(4) . . ?
C21 C26 P1 119.3(3) . . ?
C25 C26 P1 121.3(3) . . ?
C32 C31 C36 120.4(4) . . ?
C33 C32 C31 119.3(4) . . ?
C32 C33 C34 121.1(4) . . ?
C35 C34 C33 119.6(5) . . ?
C34 C35 C36 120.2(4) . . ?
C31 C36 C35 119.4(4) . . ?
C31 C36 P1 117.5(3) . . ?
C35 C36 P1 122.8(3) . . ?
C42 C41 C46 118.0(3) . . ?
C42 C41 S2 118.8(3) . . ?
C46 C41 S2 123.2(3) . . ?
C41 C42 C43 121.2(4) . . ?
C44 C43 C42 120.7(4) . . ?
C43 C44 C45 119.2(4) . . ?
C44 C45 C46 120.8(4) . . ?
C45 C46 C41 120.2(3) . . ?
C45 C46 P2 119.2(3) . . ?
C41 C46 P2 120.6(3) . . ?
C52 C51 C56 119.6(5) . . ?
C51 C52 C53 120.0(6) . . ?
C54 C53 C52 120.5(5) . . ?
C53 C54 C55 120.4(5) . . ?
C56 C55 C54 119.9(5) . . ?
C55 C56 C5l 119.6(4) . . ?
C55 C56 P2 122.6(3) . . ?
C51 C56 P2 117.8(3) . . ?
C66 C61 C62 119.8(5) . . ?
C63 C62 C61 120.4(5) . . ?
C62 C63 C64 120.2(5) . . ?
C65 C64 C63 119.7(5) . . ?
C64 C65 C66 120.8(4) . . ?
C61 C66 C65 119.1(4) . . ?
C61 C66 P2 119.0(3) . . ?
C65 C66 P2 121.3(3) . . ?
N91 C91 C92 117(3) . . ?
N93 C93 C94 151(5) . . ?
N95 C95 C96 135(4) . . ?
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
Cd O2 2.219(3) . ?
Cd Ol 2.374(3) . ?
Cd Sl 2.5082(11) . ?
Cd S2#l 2.5351(9) . ?
Cd S2 2.8700(9) . ?
S1 C11 1.758(4) . ?
S2 C41 1.787(4) . ?
S2 Cd#l 2.5351(9) . ?
Pl Ol 1.511(3) . ?
P1 C16 1.809(4) . ?
P1 C36 1.806(4) . ?
P1 C26 1.810(4) . ?
P2 O2 1.509(3) . ?
P2 C66 1.802(4) . ?
P2 C46 1.810(4) . ?
P2 C56 1.812(4) . ?
C11 C12 1.412(6) . ?
C11 C16 1.419(6) . ?
C12 C13 1.384(7) . ?
C13 C14 1.374(8) . ?
C14 C15 1.381(7) . ?
C15 C16 1.416(5) . ?
C21 C26 1.381(6) . ?
C21 C22 1.413(7) . ?
C22 C23 1.354(9) . ?
C23 C24 1.379(9) . ?
C24 C25 1.394(7) . ?
C25 C26 1.397(6) . ?
C31 C32 1.394(6) . ?
C31 C36 1.398(6) . ?
C32 C33 1.383(8) . ?
C33 C34 1.384(8) . ?
C34 C35 1.396(6) . ?
C35 C36 1.393(6) . ?
C41 C42 1.400(5) . ?
C41 C46 1.410(5) . ?
C42 C43 1.399(6) . ?
C43 C44 1.378(7) . ?
C44 C45 1.395(6) . ?
C45 C46 1.404(5) . ?
C51 C52 1.397(8) . ?
C51 C56 1.391(7) . ?
C52 C53 1.390(10) . ?
C53 C54 1.357(9) . ?
C54 C55 1.400(6) . ?
C55 C56 1.392(6) . ?
C61 C66 1.390(6) . ?
C61 C62 1.395(8) . ?
C62 C63 1.381(9) . ?
C63 C64 1.383(8) . ?
C64 C65 1.385(7) . ?
C65 C66 1.397(6) . ?
N91 C91 1.07(3) . ?
C91 C92 1.30(4) . ?
N93 C93 0.97(3) . ?
C93 C94 1.25(3) . ?
N95 C95 1.01(3) . ?
C95 C96 1.26(4) . ?
