#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:21:01 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180035 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/29/7032932.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_7032932
loop_
_publ_author_name
'Filip, I. H.'
'Gál, E'
'Lupan, I.'
'Perde-Schrepler, M'
'Lönnecke, P'
'Surducan, M.'
'Găină, L I'
'Hey-Hawkins, E'
'Silaghi-Dumitrescu, L'
_publ_section_title
;
 Tuning the coordination properties of phenothiazine by regioselective
 introduction of diphenylphosphanyl groups.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              615
_journal_page_last               629
_journal_paper_doi               10.1039/c4dt02665a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C26 H22 Cl2 N2 Pd S2'
_chemical_formula_weight         603.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-09T18:16:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.362(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1581(3)
_cell_length_b                   8.0485(2)
_cell_length_c                   15.1612(4)
_cell_measurement_reflns_used    3188
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.054
_cell_measurement_theta_min      3.29
_cell_volume                     1169.44(6)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_publication_material
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 2012, 45, 849-854.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
 SIR92
 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
 J. Appl. Crystallogr. 1993, 26, 343-350.
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0674556
_diffrn_orient_matrix_UB_12      0.0324638
_diffrn_orient_matrix_UB_13      -0.0235794
_diffrn_orient_matrix_UB_21      -0.0199372
_diffrn_orient_matrix_UB_22      -0.0173067
_diffrn_orient_matrix_UB_23      0.0396753
_diffrn_orient_matrix_UB_31      0.0230371
_diffrn_orient_matrix_UB_32      0.0800778
_diffrn_orient_matrix_UB_33      0.0181413
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8742
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.848
_exptl_absorpt_coefficient_mu    1.22
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.99342
_exptl_absorpt_correction_type   multi-scan
_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)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         3575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0277P)²+0.0830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                2863
_reflns_number_total             3575
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt02665a2.cif
_cod_data_source_block           compound_5_x1844fin
_cod_depositor_comments
'Adding full bibliography for 7032932--7032937.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7032932
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_calc_flag
Pd1 Pd 0.5 0 1 0.01213(7) Uani 1 d
Cl1 Cl 0.58515(6) 0.23363(8) 1.08892(4) 0.01972(13) Uani 1 d
S1 S 0.68166(6) 0.04612(7) 0.94154(4) 0.01382(12) Uani 1 d
N1 N 0.7717(2) -0.3114(2) 0.97057(15) 0.0175(4) Uani 1 d
C1 C 0.6772(2) -0.0971(3) 0.85323(17) 0.0151(5) Uani 1 d
C2 C 0.7227(3) -0.2610(3) 0.87718(18) 0.0167(5) Uani 1 d
C3 C 0.7193(3) -0.3696(3) 0.80468(19) 0.0215(5) Uani 1 d
H3 H 0.75 -0.4811 0.8184 0.026 Uiso 1 calc
C4 C 0.6710(3) -0.3150(4) 0.7122(2) 0.0257(6) Uani 1 d
H4 H 0.6701 -0.3899 0.6636 0.031 Uiso 1 calc
C5 C 0.6242(3) -0.1543(4) 0.68982(18) 0.0240(6) Uani 1 d
H5 H 0.5898 -0.1196 0.6264 0.029 Uiso 1 calc
C6 C 0.6280(3) -0.0441(3) 0.76078(18) 0.0203(5) Uani 1 d
H6 H 0.5972 0.0672 0.7464 0.024 Uiso 1 calc
C7 C 0.8291(3) -0.0314(3) 1.03137(17) 0.0148(5) Uani 1 d
C8 C 0.8540(2) -0.2029(3) 1.03825(17) 0.0151(5) Uani 1 d
C9 C 0.9645(3) -0.2593(3) 1.11559(18) 0.0205(5) Uani 1 d
H9 H 0.984 -0.3749 1.1226 0.025 Uiso 1 calc
C10 C 1.0455(3) -0.1501(4) 1.18168(18) 0.0231(6) Uani 1 d
H10 H 1.119 -0.1912 1.2339 0.028 Uiso 1 calc
C11 C 1.0198(3) 0.0199(3) 1.17212(18) 0.0222(6) Uani 1 d
H11 H 1.0761 0.0952 1.2172 0.027 Uiso 1 calc
C12 C 0.9116(3) 0.0781(3) 1.09635(18) 0.0179(5) Uani 1 d
H12 H 0.8939 0.194 1.089 0.021 Uiso 1 calc
C13 C 0.7763(3) -0.4881(3) 0.9910(2) 0.0256(6) Uani 1 d
H13A H 0.8604 -0.5366 0.9834 0.038 Uiso 1 calc
H13B H 0.6935 -0.5423 0.9479 0.038 Uiso 1 calc
H13C H 0.7782 -0.5046 1.0554 0.038 Uiso 1 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 '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'
S S 0.1246 0.1234 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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
Cl1 Pd1 Cl1 180 . 3_657
Cl1 Pd1 S1 84.35(2) . .
Cl1 Pd1 S1 95.65(2) 3_657 .
Cl1 Pd1 S1 95.65(2) . 3_657
Cl1 Pd1 S1 84.35(2) 3_657 3_657
S1 Pd1 S1 180.00(3) . 3_657
C1 S1 C7 98.99(11) . .
C1 S1 Pd1 111.26(8) . .
C7 S1 Pd1 103.06(8) . .
C8 N1 C2 119.3(2) . .
C8 N1 C13 119.2(2) . .
C2 N1 C13 118.4(2) . .
C6 C1 C2 121.8(2) . .
C6 C1 S1 118.46(19) . .
C2 C1 S1 119.75(19) . .
C3 C2 N1 121.6(2) . .
C3 C2 C1 117.7(2) . .
N1 C2 C1 120.7(2) . .
C4 C3 C2 120.2(3) . .
C4 C3 H3 119.9 . .
C2 C3 H3 119.9 . .
C5 C4 C3 121.4(3) . .
C5 C4 H4 119.3 . .
C3 C4 H4 119.3 . .
C4 C5 C6 119.3(3) . .
C4 C5 H5 120.3 . .
C6 C5 H5 120.3 . .
C5 C6 C1 119.6(3) . .
C5 C6 H6 120.2 . .
C1 C6 H6 120.2 . .
C12 C7 C8 121.6(2) . .
C12 C7 S1 118.87(19) . .
C8 C7 S1 119.39(18) . .
N1 C8 C7 120.8(2) . .
N1 C8 C9 122.0(2) . .
C7 C8 C9 117.1(2) . .
C10 C9 C8 121.3(2) . .
C10 C9 H9 119.3 . .
C8 C9 H9 119.3 . .
C9 C10 C11 120.3(2) . .
C9 C10 H10 119.9 . .
C11 C10 H10 119.9 . .
C12 C11 C10 119.3(2) . .
C12 C11 H11 120.3 . .
C10 C11 H11 120.3 . .
C7 C12 C11 120.3(2) . .
C7 C12 H12 119.8 . .
C11 C12 H12 119.8 . .
N1 C13 H13A 109.5 . .
N1 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
N1 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Cl1 2.3083(6) .
Pd1 Cl1 2.3083(6) 3_657
Pd1 S1 2.3267(6) .
Pd1 S1 2.3267(6) 3_657
S1 C1 1.756(2) .
S1 C7 1.770(2) .
N1 C8 1.395(3) .
N1 C2 1.396(3) .
N1 C13 1.452(3) .
C1 C6 1.390(3) .
C1 C2 1.405(3) .
C2 C3 1.396(3) .
C3 C4 1.394(4) .
C3 H3 0.95 .
C4 C5 1.381(4) .
C4 H4 0.95 .
C5 C6 1.385(4) .
C5 H5 0.95 .
C6 H6 0.95 .
C7 C12 1.379(3) .
C7 C8 1.401(3) .
C8 C9 1.403(3) .
C9 C10 1.381(4) .
C9 H9 0.95 .
C10 C11 1.391(4) .
C10 H10 0.95 .
C11 C12 1.382(4) .
C11 H11 0.95 .
C12 H12 0.95 .
C13 H13A 0.98 .
C13 H13B 0.98 .
C13 H13C 0.98 .
