#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:00:41 +0200 (dom 07 de ago de 2016) $
#$Revision: 185404 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/92/7039283.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_7039283
loop_
_publ_author_name
'Poirier, Stéphanie'
'Tailleur, Elodie'
'Lynn, Hudson'
'Reber, Christian'
_publ_section_title
;
 Characterization of PdH-C interactions in bis-dimethyldithiocarbamate
 palladium(ii) and its deuterated analog by luminescence spectroscopy at
 variable pressure.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10883
_journal_page_last               10886
_journal_paper_doi               10.1039/c6dt01574c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C6 D12 N2 Pd S4'
_chemical_formula_sum            'C6 D12 N2 Pd S4'
_chemical_formula_weight         358.89
_chemical_name_systematic
'bis-d12-dimethyldithiocarbamate palldium(II)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2015-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-04-18 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                65.235(6)
_cell_angle_beta                 67.183(7)
_cell_angle_gamma                84.974(7)
_cell_formula_units_Z            1
_cell_length_a                   6.4754(14)
_cell_length_b                   7.0391(15)
_cell_length_c                   7.6797(16)
_cell_measurement_reflns_used    6707
_cell_measurement_temperature    295
_cell_measurement_theta_max      60.856
_cell_measurement_theta_min      6.050
_cell_volume                     291.81(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      295
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5927
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.826
_diffrn_reflns_theta_min         6.048
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    12.709
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.2130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1693 before and 0.0908 after correction.
The Ratio of minimum to maximum transmission is 0.2833.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             172
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       0.23(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0841P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1285
_reflns_number_total             1289
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;

    rebe68.res created by SHELXL-2014/7

TITL rebe68_a.res in P-1
REM Old TITL rebe68 in P1 #1
REM SHELXT solution in P-1
REM R1 0.087, Rweak 0.022, Alpha 0.069, Orientation as input
REM Formula found by SHELXT: C4 N4 S4 Pd
CELL 1.34139 6.4754 7.0391 7.6797 65.235 67.183 84.974
ZERR 1 0.0014 0.0015 0.0016 0.006 0.007 0.007
LATT 1
SFAC C D N Pd S
DISP C 0.015 0.007 57.748
DISP D -0 0
DISP N 0.025 0.014 110.512
DISP Pd 0.066 3.131 23543.655
DISP S 0.292 0.425 3241.763
UNIT 6 12 2 1 4
 
L.S. 10
PLAN  5
SIZE 0.06 0.24 0.32
TEMP 22
BOND $H
ACTA
fmap 2
MORE -1
CONF
REM <olex2.extras>
REM <HklSrc "%.\\rebe68.hkl">
REM </olex2.extras>
 
WGHT    0.084100
EXTI    0.232613
FVAR       1.73594
PD    4    0.000000    0.000000    1.000000    10.50000    0.04244    0.04223 =
         0.04262   -0.01627   -0.01595   -0.00073
S1    5    0.317897    0.206467    0.913296    11.00000    0.04563    0.04709 =
         0.05774   -0.01613   -0.02350    0.00010
S2    5   -0.065442    0.337341    0.811704    11.00000    0.04698    0.04590 =
         0.05830   -0.01539   -0.02511   -0.00068
C3    1    0.190656    0.416167    0.790540    11.00000    0.04149    0.04655 =
         0.04215   -0.01750   -0.01458    0.00002
N1    3    0.277972    0.610312    0.691573    11.00000    0.04600    0.04761 =
         0.05011   -0.01684   -0.01876   -0.00263
C1    1    0.492416    0.670020    0.685018    11.00000    0.04796    0.05758 =
         0.07080   -0.02014   -0.02030   -0.00988
AFIX 137
D1A   2    0.466842    0.752394    0.763177    11.00000   -1.50000
D1B   2    0.590615    0.751064    0.543229    11.00000   -1.50000
D1C   2    0.560594    0.545805    0.744343    11.00000   -1.50000
AFIX   0
C2    1    0.162246    0.780673    0.589915    11.00000    0.06394    0.04612 =
         0.05995   -0.01761   -0.02422    0.00331
AFIX 137
D2A   2    0.026173    0.723913    0.600492    11.00000   -1.50000
D2B   2    0.257898    0.855256    0.445910    11.00000   -1.50000
D2C   2    0.126384    0.875146    0.656335    11.00000   -1.50000
AFIX   0
HKLF 4
 
REM  rebe68_a.res in P-1
REM R1 =  0.0523 for    1285 Fo > 4sig(Fo)  and  0.0523 for all    1289 data
REM     64 parameters refined using      0 restraints
 
END  
     
WGHT      0.0841      0.0000 

REM Highest difference peak  0.994,  deepest hole -1.135,  1-sigma level  0.260
Q1    1   0.0225  0.2358  0.7708  11.00000  0.05    0.99
Q2    1   0.1388  0.2073  0.8661  11.00000  0.05    0.99
Q3    1  -0.2275  0.3213  0.7607  11.00000  0.05    0.73
Q4    1   0.1177  0.3924  0.7840  11.00000  0.05    0.73
Q5    1   0.4926  0.4158  0.7339  11.00000  0.05    0.73

REM The information below was added by Olex2.
REM
REM R1 = 0.0523 for 1285 Fo > 4sig(Fo) and 0.0523 for all 5927 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.99, deepest hole -1.14
REM Mean Shift 0, Max Shift 0.000.

REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0523
REM R1_gt = 0.0523
REM wR_ref = 0.1190
REM GOOF = 1.264
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 5927
REM Reflections_gt = 1285
REM Parameters = n/a
REM Hole = -1.14
REM Peak = 0.99
REM Flack = n/a

;
_cod_data_source_file            c6dt01574c2.cif
_cod_data_source_block           rebe68
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039283--7039284.cif.
;
_cod_database_code               7039283
_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.
;
_shelx_estimated_absorpt_t_max   0.516
_shelx_estimated_absorpt_t_min   0.106
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(D1A,D1B,D1C), C2(D2A,D2B,D2C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Acetone
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd Pd 0.0000 0.0000 1.0000 0.0429(3) Uani 1 2 d S T P
S1 S 0.31790(16) 0.20647(16) 0.91330(16) 0.0509(3) Uani 1 1 d . . .
S2 S -0.06544(16) 0.33734(15) 0.81170(17) 0.0509(3) Uani 1 1 d . . .
C3 C 0.1907(6) 0.4162(6) 0.7905(6) 0.0441(7) Uani 1 1 d . . .
N1 N 0.2780(5) 0.6103(5) 0.6916(5) 0.0487(7) Uani 1 1 d . . .
C1 C 0.4924(7) 0.6700(7) 0.6850(8) 0.0612(10) Uani 1 1 d . . .
D1A D 0.4668 0.7524 0.7632 0.092 Uiso 1 1 calc GR . .
D1B D 0.5906 0.7511 0.5432 0.092 Uiso 1 1 calc GR . .
D1C D 0.5606 0.5458 0.7443 0.092 Uiso 1 1 calc GR . .
C2 C 0.1622(8) 0.7807(7) 0.5899(8) 0.0582(9) Uani 1 1 d . . .
D2A D 0.0262 0.7239 0.6005 0.087 Uiso 1 1 calc GR . .
D2B D 0.2579 0.8553 0.4459 0.087 Uiso 1 1 calc GR . .
D2C D 0.1264 0.8751 0.6563 0.087 Uiso 1 1 calc GR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd 0.0424(3) 0.0422(3) 0.0426(3) -0.0163(2) -0.0160(2) -0.00073(17)
S1 0.0456(5) 0.0471(5) 0.0577(6) -0.0161(4) -0.0235(4) 0.0001(4)
S2 0.0470(5) 0.0459(5) 0.0583(6) -0.0154(4) -0.0251(4) -0.0007(4)
C3 0.0415(15) 0.0466(16) 0.0421(15) -0.0175(13) -0.0146(12) 0.0000(12)
N1 0.0460(14) 0.0476(15) 0.0501(15) -0.0168(13) -0.0188(12) -0.0026(11)
C1 0.0480(18) 0.058(2) 0.071(2) -0.0201(18) -0.0203(17) -0.0099(15)
C2 0.064(2) 0.0461(17) 0.060(2) -0.0176(15) -0.0242(17) 0.0033(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0150 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.0660 3.1310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.2920 0.4250 '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
S1 Pd S1 180.0 2_557 .
S2 Pd S1 75.73(4) 2_557 2_557
S2 Pd S1 75.73(4) . .
S2 Pd S1 104.27(4) 2_557 .
S2 Pd S1 104.27(4) . 2_557
S2 Pd S2 180.0 . 2_557
C3 S1 Pd 85.90(14) . .
C3 S2 Pd 86.73(14) . .
S2 C3 S1 111.6(2) . .
N1 C3 S1 124.4(3) . .
N1 C3 S2 123.9(3) . .
C3 N1 C1 121.7(3) . .
C3 N1 C2 121.8(3) . .
C2 N1 C1 116.4(3) . .
N1 C1 D1A 109.5 . .
N1 C1 D1B 109.5 . .
N1 C1 D1C 109.5 . .
D1A C1 D1B 109.5 . .
D1A C1 D1C 109.5 . .
D1B C1 D1C 109.5 . .
N1 C2 D2A 109.5 . .
N1 C2 D2B 109.5 . .
N1 C2 D2C 109.5 . .
D2A C2 D2B 109.5 . .
D2A C2 D2C 109.5 . .
D2B C2 D2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd S1 2.3331(10) 2_557
Pd S1 2.3331(10) .
Pd S2 2.3090(10) .
Pd S2 2.3090(10) 2_557
S1 C3 1.723(4) .
S2 C3 1.721(4) .
C3 N1 1.303(5) .
N1 C1 1.462(5) .
N1 C2 1.456(5) .
C1 D1A 0.9600 .
C1 D1B 0.9600 .
C1 D1C 0.9600 .
C2 D2A 0.9600 .
C2 D2B 0.9600 .
C2 D2C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Pd S1 C3 S2 -0.38(19)
Pd S1 C3 N1 -179.6(4)
Pd S2 C3 S1 0.4(2)
Pd S2 C3 N1 179.6(4)
S1 C3 N1 C1 -3.3(6)
S1 C3 N1 C2 179.7(3)
S2 C3 N1 C1 177.6(3)
S2 C3 N1 C2 0.5(6)
