#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:06:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179826 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/22/7012233.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_7012233
loop_
_publ_author_name
'Dervisi, Athanasia'
'Jenkins, Robert L.'
'Malik, K. M. Abdul'
'Hursthouse, Michael B.'
'Coles, Simon'
_publ_section_title
;
 Synthesis of Ni(ii), Pd(ii) and Pt(ii) complexes containing chiral
 phosphino-thiol and -thioether ligands
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1133
_journal_paper_doi               10.1039/b209142a
_journal_year                    2003
_chemical_formula_sum            'C17 H21 Cl2 P Pd S'
_chemical_formula_weight         465.67
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8678(18)
_cell_length_b                   15.492(3)
_cell_length_c                   13.085(3)
_cell_measurement_reflns_used    19520
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1789.4(7)
_computing_cell_refinement       'DENZO, COLLECT'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) & Collect (Hooft, 1998)'
_computing_data_reduction        'DENZO, COLLECT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD Area Detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24775
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  0.8870
_exptl_absorpt_correction_T_min  0.7488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.944
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.0020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[σ²(Fo²)+(0.0627P)²+0.3583P] where 
P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                3669
_reflns_number_total             4094
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b209142a.txt
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1789.4(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012233
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.2062(3) -0.10088(16) 0.14213(19) 0.0237(5) Uani 1 1 d . . .
H1 H -0.2103 -0.1097 0.2175 0.028 Uiso 1 1 calc R . .
C2 C -0.3043(3) -0.17059(17) 0.0841(2) 0.0272(6) Uani 1 1 d . . .
H2A H -0.2688 -0.2278 0.1100 0.033 Uiso 1 1 calc R . .
H2B H -0.4100 -0.1635 0.1011 0.033 Uiso 1 1 calc R . .
C3 C -0.3048(3) -0.1706(2) -0.0313(2) 0.0354(7) Uani 1 1 d . . .
H3A H -0.3429 -0.1150 -0.0587 0.053 Uiso 1 1 calc R . .
H3B H -0.3703 -0.2171 -0.0604 0.053 Uiso 1 1 calc R . .
H3C H -0.2014 -0.1796 -0.0498 0.053 Uiso 1 1 calc R . .
C4 C -0.2546(3) -0.00933(16) 0.1157(2) 0.0239(6) Uani 1 1 d . . .
H4A H -0.3610 -0.0003 0.1302 0.029 Uiso 1 1 calc R . .
H4B H -0.2471 0.0019 0.0419 0.029 Uiso 1 1 calc R . .
C5 C -0.1988(3) 0.07020(14) 0.32038(18) 0.0180(5) Uani 1 1 d . . .
C6 C -0.3548(3) 0.07367(16) 0.3288(2) 0.0236(5) Uani 1 1 d . . .
H6 H -0.4243 0.0713 0.2689 0.028 Uiso 1 1 calc R . .
C7 C -0.4075(3) 0.08058(17) 0.4249(2) 0.0275(6) Uani 1 1 d . . .
H7 H -0.5134 0.0815 0.4306 0.033 Uiso 1 1 calc R . .
C8 C -0.3072(3) 0.08619(18) 0.5126(2) 0.0290(6) Uani 1 1 d . . .
H8 H -0.3440 0.0915 0.5781 0.035 Uiso 1 1 calc R . .
C9 C -0.1528(3) 0.08393(18) 0.5040(2) 0.0285(6) Uani 1 1 d . . .
H9 H -0.0836 0.0882 0.5639 0.034 Uiso 1 1 calc R . .
C10 C -0.0980(3) 0.07546(16) 0.40843(19) 0.0228(5) Uani 1 1 d . . .
H10 H 0.0080 0.0733 0.4033 0.027 Uiso 1 1 calc R . .
C11 C -0.1653(3) 0.17037(15) 0.13958(17) 0.0176(5) Uani 1 1 d . . .
C12 C -0.2750(3) 0.18287(17) 0.0565(2) 0.0264(6) Uani 1 1 d . . .
H12 H -0.3287 0.1348 0.0261 0.032 Uiso 1 1 calc R . .
C13 C -0.3051(3) 0.26501(18) 0.0187(2) 0.0314(6) Uani 1 1 d . . .
H13 H -0.3797 0.2730 -0.0376 0.038 Uiso 1 1 calc R . .
C14 C -0.2279(3) 0.33589(17) 0.0622(2) 0.0258(5) Uani 1 1 d . . .
H14 H -0.2498 0.3922 0.0362 0.031 Uiso 1 1 calc R . .
C15 C -0.1184(3) 0.32378(16) 0.14374(19) 0.0219(5) Uani 1 1 d . . .
H15 H -0.0644 0.3720 0.1733 0.026 Uiso 1 1 calc R . .
C16 C -0.0872(3) 0.24188(16) 0.18253(18) 0.0203(5) Uani 1 1 d . . .
H16 H -0.0121 0.2343 0.2387 0.024 Uiso 1 1 calc R . .
C17 C 0.0499(4) -0.2014(2) 0.1909(3) 0.0507(9) Uani 1 1 d . . .
H17A H 0.0127 -0.1956 0.2587 0.076 Uiso 1 1 calc R . .
H17B H 0.1607 -0.2056 0.1987 0.076 Uiso 1 1 calc R . .
H17C H 0.0071 -0.2537 0.1573 0.076 Uiso 1 1 calc R . .
P1 P -0.12888(6) 0.06436(4) 0.19436(5) 0.01624(15) Uani 1 1 d . . .
S1 S -0.00685(7) -0.10807(4) 0.11345(5) 0.02293(16) Uani 1 1 d . . .
Cl1 Cl 0.34235(6) -0.05812(4) 0.17990(5) 0.02500(15) Uani 1 1 d . . .
Cl2 Cl 0.21998(6) 0.12283(4) 0.28283(5) 0.02428(15) Uani 1 1 d . . .
Pd1 Pd 0.104423(18) 0.008175(11) 0.194753(12) 0.01454(10) 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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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'
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
C4 C1 C2 114.3(2) . . ?
C4 C1 S1 105.44(17) . . ?
C2 C1 S1 111.35(17) . . ?
C3 C2 C1 116.1(2) . . ?
C1 C4 P1 108.13(18) . . ?
C10 C5 C6 119.6(2) . . ?
C10 C5 P1 120.39(17) . . ?
C6 C5 P1 119.93(19) . . ?
C7 C6 C5 119.7(2) . . ?
C8 C7 C6 120.7(2) . . ?
C7 C8 C9 119.5(2) . . ?
C8 C9 C10 120.6(3) . . ?
C9 C10 C5 119.9(2) . . ?
C16 C11 C12 118.9(2) . . ?
C16 C11 P1 119.88(18) . . ?
C12 C11 P1 121.16(18) . . ?
C13 C12 C11 120.1(2) . . ?
C12 C13 C14 120.8(2) . . ?
C15 C14 C13 119.4(2) . . ?
C14 C15 C16 120.5(2) . . ?
C15 C16 C11 120.4(2) . . ?
C11 P1 C5 104.51(10) . . ?
C11 P1 C4 105.45(11) . . ?
C5 P1 C4 107.27(12) . . ?
C11 P1 Pd1 118.88(8) . . ?
C5 P1 Pd1 114.30(8) . . ?
C4 P1 Pd1 105.64(9) . . ?
C17 S1 C1 98.90(15) . . ?
C17 S1 Pd1 106.66(12) . . ?
C1 S1 Pd1 103.82(8) . . ?
P1 Pd1 S1 86.98(3) . . ?
P1 Pd1 Cl2 93.89(3) . . ?
S1 Pd1 Cl2 177.75(2) . . ?
P1 Pd1 Cl1 174.37(2) . . ?
S1 Pd1 Cl1 88.18(3) . . ?
Cl2 Pd1 Cl1 91.05(3) . . ?
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
C1 C4 1.512(4) . ?
C1 C2 1.541(4) . ?
C1 S1 1.846(3) . ?
C2 C3 1.510(4) . ?
C4 P1 1.840(3) . ?
C5 C10 1.391(3) . ?
C5 C6 1.399(3) . ?
C5 P1 1.819(2) . ?
C6 C7 1.386(4) . ?
C7 C8 1.386(4) . ?
C8 C9 1.385(4) . ?
C9 C10 1.390(4) . ?
C11 C16 1.396(3) . ?
C11 C12 1.401(3) . ?
C11 P1 1.809(2) . ?
C12 C13 1.382(4) . ?
C13 C14 1.387(4) . ?
C14 C15 1.385(4) . ?
C15 C16 1.385(3) . ?
C17 S1 1.810(3) . ?
P1 Pd1 2.2441(7) . ?
S1 Pd1 2.2688(7) . ?
Cl1 Pd1 2.3713(7) . ?
Cl2 Pd1 2.3037(7) . ?
