#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/28/4342809.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_4342809
loop_
_publ_author_name
'Sherwood, Rebecca'
'Gonzàlez de Rivera, Ferran'
'Wan, Jane Hui'
'Zhang, Qi'
'White, Andrew J. P.'
'Rossell, Oriol'
'Hogarth, Graeme'
'Wilton-Ely, James D E T'
_publ_section_title
;
 Multimetallic complexes based on a diphosphine-dithiocarbamate
 "janus" ligand.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4222
_journal_page_last               4230
_journal_paper_doi               10.1021/ic5028527
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C58 H56 N2 P4 Pd2 S4, 2(Cl), 2(H2 O), 1.5(C H4 O)'
_chemical_formula_sum            'C59.5 H66 Cl2 N2 O3.5 P4 Pd2 S4'
_chemical_formula_weight         1400.96
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 100.016(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4321(3)
_cell_length_b                   17.1025(5)
_cell_length_c                   15.3940(5)
_cell_measurement_reflns_used    8995
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.2310
_cell_measurement_theta_min      2.6930
_cell_volume                     2963.92(15)
_computing_cell_refinement       CrysAlisPro,
_computing_data_collection       CrysAlisPro,
_computing_data_reduction        CrysAlisPro,
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.615
_diffrn_reflns_theta_min         2.434
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1430
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
 H2O protons on O(40) not located so, asu 2H and UNIT 8H low
 
 SQUEEZE suggested 56 e/cell = 14 e/asu
 The solvents used were MeOH (CH4O, 18e) and dcm (CH2Cl2, 42e).
 Before the use of SQUEEZE the solvent most resembled MeOH
 0.75MeOH = 13.5e, so this was used as the solvent present.
 
 So, the atom list is low by 0.75(C H4 O) + 2H = C0.75 H5 O0.75,
 and the UNIT is low by C3 H20 O3, i.e. C116 H112 Cl4 N4 O4 P8 Pd4 S8
;
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0428P)²+0.7594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4736
_reflns_number_total             6482
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5028527_si_005.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 4342808--4342809.cif.'
_cod_original_cell_volume        2963.93(16)
_cod_original_formula_sum        'C59.50 H66 Cl2 N2 O3.50 P4 Pd2 S4'
_cod_database_code               4342809
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Pd1 Pd 0.11349(3) 0.12422(2) 0.49768(2) 0.01485(10) Uani 1 1 d . .
S1 S -0.09289(8) -0.06648(7) 0.36820(6) 0.0178(2) Uani 1 1 d . .
C2 C 0.0565(3) -0.0673(2) 0.4089(2) 0.0147(8) Uani 1 1 d . .
S3 S 0.09083(8) -0.12748(7) 0.49969(6) 0.0180(2) Uani 1 1 d . .
N4 N 0.1350(3) -0.0263(2) 0.3736(2) 0.0166(7) Uani 1 1 d . .
C5 C 0.0974(4) 0.0116(3) 0.2869(3) 0.0209(10) Uani 1 1 d . .
H5A H 0.0504 -0.0267 0.2471 0.025 Uiso 1 1 calc R U
H5B H 0.1697 0.0236 0.2620 0.025 Uiso 1 1 calc R U
C6 C 0.0246(4) 0.0865(3) 0.2851(3) 0.0218(10) Uani 1 1 d . .
H6A H -0.0532 0.0722 0.3003 0.026 Uiso 1 1 calc R U
H6B H 0.0092 0.1054 0.2234 0.026 Uiso 1 1 calc R U
P7 P 0.08191(9) 0.16869(7) 0.35466(7) 0.0186(2) Uani 1 1 d . .
C8 C 0.2630(3) -0.0393(2) 0.4027(3) 0.0176(9) Uani 1 1 d . .
H8A H 0.2934 -0.0704 0.3571 0.021 Uiso 1 1 calc R U
H8B H 0.2745 -0.0707 0.4575 0.021 Uiso 1 1 calc R U
C9 C 0.3365(3) 0.0354(2) 0.4197(3) 0.0173(9) Uani 1 1 d . .
H9A H 0.3233 0.0664 0.3645 0.021 Uiso 1 1 calc R U
H9B H 0.4214 0.0202 0.4312 0.021 Uiso 1 1 calc R U
P10 P 0.31097(9) 0.10030(7) 0.50961(7) 0.0164(2) Uani 1 1 d . .
C11 C -0.0407(4) 0.2379(3) 0.3416(3) 0.0246(10) Uani 1 1 d . .
C12 C -0.1378(4) 0.2329(3) 0.2733(3) 0.0361(13) Uani 1 1 d . .
H12A H -0.1396 0.1940 0.2291 0.043 Uiso 1 1 calc R U
C13 C -0.2321(5) 0.2847(4) 0.2699(4) 0.0479(16) Uani 1 1 d . .
H13A H -0.2989 0.2799 0.2240 0.057 Uiso 1 1 calc R U
C14 C -0.2304(5) 0.3429(4) 0.3317(4) 0.0484(16) Uani 1 1 d . .
H14A H -0.2952 0.3782 0.3284 0.058 Uiso 1 1 calc R U
C15 C -0.1348(5) 0.3494(3) 0.3977(4) 0.0476(16) Uani 1 1 d . .
H15A H -0.1327 0.3903 0.4398 0.057 Uiso 1 1 calc R U
C16 C -0.0394(4) 0.2968(3) 0.4047(3) 0.0352(12) Uani 1 1 d . .
H16A H 0.0257 0.3012 0.4521 0.042 Uiso 1 1 calc R U
C17 C 0.1968(4) 0.2142(3) 0.3042(3) 0.0205(9) Uani 1 1 d . .
C18 C 0.2372(4) 0.1813(3) 0.2320(3) 0.0264(10) Uani 1 1 d . .
H18A H 0.2022 0.1345 0.2062 0.032 Uiso 1 1 calc R U
C19 C 0.3290(4) 0.2169(3) 0.1979(3) 0.0325(12) Uani 1 1 d . .
H19A H 0.3560 0.1943 0.1486 0.039 Uiso 1 1 calc R U
C20 C 0.3807(4) 0.2841(3) 0.2345(3) 0.0333(12) Uani 1 1 d . .
H20A H 0.4444 0.3072 0.2114 0.040 Uiso 1 1 calc R U
C21 C 0.3398(4) 0.3186(3) 0.3058(3) 0.0323(12) Uani 1 1 d . .
H21A H 0.3748 0.3655 0.3311 0.039 Uiso 1 1 calc R U
C22 C 0.2479(4) 0.2838(3) 0.3392(3) 0.0251(10) Uani 1 1 d . .
H22A H 0.2191 0.3078 0.3870 0.030 Uiso 1 1 calc R U
C23 C 0.4064(3) 0.1827(3) 0.5016(3) 0.0207(10) Uani 1 1 d . .
C24 C 0.5107(4) 0.1755(3) 0.4669(3) 0.0277(11) Uani 1 1 d . .
H24A H 0.5285 0.1275 0.4409 0.033 Uiso 1 1 calc R U
C25 C 0.5882(4) 0.2380(3) 0.4703(3) 0.0370(13) Uani 1 1 d . .
H25A H 0.6591 0.2327 0.4464 0.044 Uiso 1 1 calc R U
C26 C 0.5635(4) 0.3076(3) 0.5079(3) 0.0383(13) Uani 1 1 d . .
H26A H 0.6180 0.3498 0.5107 0.046 Uiso 1 1 calc R U
C27 C 0.4594(4) 0.3165(3) 0.5418(3) 0.0336(12) Uani 1 1 d . .
H27A H 0.4420 0.3651 0.5668 0.040 Uiso 1 1 calc R U
C28 C 0.3805(4) 0.2539(3) 0.5392(3) 0.0252(10) Uani 1 1 d . .
H28A H 0.3095 0.2595 0.5628 0.030 Uiso 1 1 calc R U
C29 C 0.3798(3) 0.0536(2) 0.6121(3) 0.0170(9) Uani 1 1 d . .
C30 C 0.4704(3) 0.0906(3) 0.6716(3) 0.0207(9) Uani 1 1 d . .
H30A H 0.4950 0.1418 0.6588 0.025 Uiso 1 1 calc R U
C31 C 0.5241(4) 0.0540(3) 0.7478(3) 0.0264(11) Uani 1 1 d . .
H31A H 0.5855 0.0797 0.7870 0.032 Uiso 1 1 calc R U
C32 C 0.4887(4) -0.0195(3) 0.7671(3) 0.0313(12) Uani 1 1 d . .
H32A H 0.5281 -0.0455 0.8186 0.038 Uiso 1 1 calc R U
C33 C 0.3963(4) -0.0564(3) 0.7125(3) 0.0284(11) Uani 1 1 d . .
H33A H 0.3706 -0.1066 0.7275 0.034 Uiso 1 1 calc R U
C34 C 0.3414(4) -0.0199(3) 0.6361(3) 0.0225(10) Uani 1 1 d . .
H34A H 0.2768 -0.0449 0.5994 0.027 Uiso 1 1 calc R U
Cl1 Cl 0.28039(13) 0.50630(9) 0.41580(9) 0.0508(4) Uani 1 1 d . .
O40 O 0.4449(4) 0.5155(2) 0.6016(2) 0.0519(11) 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'
Cl Cl 0.1484 0.1585 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
P10 Pd1 P7 97.21(4) . .
P10 Pd1 S1 95.97(4) . 3_556
P7 Pd1 S1 164.39(4) . 3_556
P10 Pd1 S3 169.39(4) . 3_556
P7 Pd1 S3 91.02(4) . 3_556
S1 Pd1 S3 74.99(3) 3_556 3_556
C2 S1 Pd1 85.46(13) . 3_556
N4 C2 S1 123.2(3) . .
N4 C2 S3 124.9(3) . .
S1 C2 S3 111.9(2) . .
C2 S3 Pd1 85.00(13) . 3_556
C2 N4 C8 120.2(3) . .
C2 N4 C5 119.4(3) . .
C8 N4 C5 117.2(3) . .
N4 C5 C6 117.2(3) . .
C5 C6 P7 119.9(3) . .
C17 P7 C6 107.00(19) . .
C17 P7 C11 105.95(19) . .
C6 P7 C11 104.3(2) . .
C17 P7 Pd1 123.23(14) . .
C6 P7 Pd1 106.79(14) . .
C11 P7 Pd1 108.11(14) . .
N4 C8 C9 114.5(3) . .
C8 C9 P10 118.6(3) . .
C23 P10 C29 103.13(19) . .
C23 P10 C9 104.10(18) . .
C29 P10 C9 106.70(19) . .
C23 P10 Pd1 117.34(15) . .
C29 P10 Pd1 115.01(12) . .
C9 P10 Pd1 109.53(13) . .
C12 C11 C16 118.7(4) . .
C12 C11 P7 122.8(4) . .
C16 C11 P7 118.5(4) . .
C13 C12 C11 120.1(5) . .
C14 C13 C12 121.2(5) . .
C15 C14 C13 119.3(5) . .
C14 C15 C16 121.1(6) . .
C11 C16 C15 119.6(5) . .
C22 C17 C18 118.6(4) . .
C22 C17 P7 119.1(3) . .
C18 C17 P7 122.3(3) . .
C19 C18 C17 120.0(4) . .
C20 C19 C18 120.8(4) . .
C19 C20 C21 119.9(4) . .
C22 C21 C20 119.4(5) . .
C21 C22 C17 121.3(4) . .
C24 C23 C28 119.4(4) . .
C24 C23 P10 121.7(4) . .
C28 C23 P10 118.6(3) . .
C25 C24 C23 120.1(5) . .
C26 C25 C24 120.5(5) . .
C25 C26 C27 120.5(5) . .
C26 C27 C28 119.7(5) . .
C27 C28 C23 119.8(4) . .
C34 C29 C30 117.4(4) . .
C34 C29 P10 120.9(3) . .
C30 C29 P10 121.6(3) . .
C31 C30 C29 121.2(4) . .
C32 C31 C30 119.9(4) . .
C31 C32 C33 120.7(4) . .
C34 C33 C32 119.9(4) . .
C33 C34 C29 120.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 P10 2.2702(10) .
Pd1 P7 2.2978(11) .
Pd1 S1 2.3371(10) 3_556
Pd1 S3 2.3438(10) 3_556
S1 C2 1.714(4) .
S1 Pd1 2.3372(10) 3_556
C2 N4 1.327(5) .
C2 S3 1.725(4) .
S3 Pd1 2.3438(10) 3_556
N4 C8 1.471(5) .
N4 C5 1.479(5) .
C5 C6 1.525(6) .
C6 P7 1.819(5) .
P7 C17 1.813(4) .
P7 C11 1.819(4) .
C8 C9 1.528(5) .
C9 P10 1.837(4) .
P10 C23 1.800(4) .
P10 C29 1.821(4) .
C11 C12 1.392(6) .
C11 C16 1.398(7) .
C12 C13 1.389(7) .
C13 C14 1.374(8) .
C14 C15 1.361(8) .
C15 C16 1.404(7) .
C17 C22 1.393(6) .
C17 C18 1.394(6) .
C18 C19 1.393(6) .
C19 C20 1.368(7) .
C20 C21 1.396(7) .
C21 C22 1.382(6) .
C23 C24 1.394(6) .
C23 C28 1.401(6) .
C24 C25 1.384(6) .
C25 C26 1.375(7) .
C26 C27 1.388(7) .
C27 C28 1.397(6) .
C29 C34 1.402(6) .
C29 C30 1.407(6) .
C30 C31 1.377(6) .
C31 C32 1.370(7) .
C32 C33 1.382(6) .
C33 C34 1.382(6) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.500 114 28 ' '
2 0.500 1.000 1.000 114 28 ' '
