Multimetallic complexes based on a diphosphine-dithiocarbamate "janus" ligand.
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; Inorganic chemistry 54 (2015) 4222–4230; doi:10.1021/ic5028527

data_4342809
_publ_section_title
;
 Multimetallic complexes based on a diphosphine-dithiocarbamate
 &quot;janus&quot; 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/[\s^2^(Fo^2^)+(0.0428P)^2^+0.7594P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_shelxl_version_number           2013-4