#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:17:28 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180498 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/67/7216754.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_7216754
loop_
_publ_author_name
'Copolovici, Dana'
'Isaia, Francesco'
'Breunig, Hans J.'
'Raţ, Ciprian I.'
'Silvestru, Cristian'
_publ_section_title
;
 Palladium(ii) complexes with chiral organoantimony(iii) ligands. Solution
 behaviour and solid state structures
;
_journal_issue                   51
_journal_name_full               'RSC Advances'
_journal_page_first              26569
_journal_paper_doi               10.1039/c4ra03482a
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C27 H34 Cl2 N Pd Sb'
_chemical_formula_sum            'C27 H34 Cl2 N Pd Sb'
_chemical_formula_weight         671.60
_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                 107.6790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3725(7)
_cell_length_b                   23.1231(18)
_cell_length_c                   12.9278(10)
_cell_measurement_reflns_used    4963
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      23.75
_cell_measurement_theta_min      2.38
_cell_volume                     2669.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19169
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  0.8628
_exptl_absorpt_correction_T_min  0.7023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, 2001.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0301P)²+3.5047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                4303
_reflns_number_total             4704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra03482a2.cif
_cod_data_source_block           307rich
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7216754
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
C1 C 0.0630(5) 0.08945(19) 0.1970(4) 0.0299(10) Uani 1 1 d .
C2 C 0.0038(5) 0.1053(2) 0.2797(4) 0.0344(11) Uani 1 1 d .
C3 C -0.1196(6) 0.0750(2) 0.2884(4) 0.0469(13) Uani 1 1 d .
H3 H -0.1618 0.0853 0.3423 0.056 Uiso 1 1 calc R
C4 C -0.1812(6) 0.0301(2) 0.2191(5) 0.0503(14) Uani 1 1 d .
H4 H -0.2625 0.0098 0.2279 0.060 Uiso 1 1 calc R
C5 C -0.1236(6) 0.0153(2) 0.1381(4) 0.0450(13) Uani 1 1 d .
H5 H -0.1654 -0.0148 0.0910 0.054 Uiso 1 1 calc R
C6 C -0.0029(6) 0.0454(2) 0.1264(4) 0.0407(12) Uani 1 1 d .
H6 H 0.0351 0.0359 0.0700 0.049 Uiso 1 1 calc R
C7 C 0.0702(6) 0.1523(2) 0.3609(4) 0.0386(12) Uani 1 1 d .
H7A H 0.0265 0.1493 0.4198 0.046 Uiso 1 1 calc R
H7B H 0.1767 0.1450 0.3912 0.046 Uiso 1 1 calc R
C8 C -0.1131(6) 0.2240(3) 0.2628(5) 0.0608(17) Uani 1 1 d .
H8A H -0.1695 0.2159 0.3119 0.091 Uiso 1 1 calc R
H8B H -0.1463 0.1991 0.2006 0.091 Uiso 1 1 calc R
H8C H -0.1279 0.2636 0.2397 0.091 Uiso 1 1 calc R
C9 C 0.0967(7) 0.2508(2) 0.4170(4) 0.0572(16) Uani 1 1 d .
H9A H 0.0875 0.2907 0.3956 0.086 Uiso 1 1 calc R
H9B H 0.1990 0.2425 0.4569 0.086 Uiso 1 1 calc R
H9C H 0.0340 0.2432 0.4619 0.086 Uiso 1 1 calc R
C10 C 0.2260(5) 0.13028(18) 0.0111(3) 0.0277(10) Uani 1 1 d .
C11 C 0.0851(5) 0.14205(19) -0.0631(4) 0.0327(11) Uani 1 1 d .
C12 C 0.0700(6) 0.1386(2) -0.1732(4) 0.0394(12) Uani 1 1 d .
H12 H -0.0238 0.1450 -0.2228 0.047 Uiso 1 1 calc R
C13 C 0.1888(6) 0.1261(2) -0.2119(4) 0.0384(12) Uani 1 1 d .
C14 C 0.3281(6) 0.1171(2) -0.1369(4) 0.0361(11) Uani 1 1 d .
H14 H 0.4095 0.1093 -0.1616 0.043 Uiso 1 1 calc R
C15 C 0.3495(5) 0.1193(2) -0.0256(4) 0.0317(10) Uani 1 1 d .
C16 C -0.0498(5) 0.1617(2) -0.0332(4) 0.0437(13) Uani 1 1 d .
H16A H -0.1230 0.1771 -0.0963 0.066 Uiso 1 1 calc R
H16B H -0.0208 0.1912 0.0216 0.066 Uiso 1 1 calc R
H16C H -0.0919 0.1295 -0.0057 0.066 Uiso 1 1 calc R
C17 C 0.1679(8) 0.1233(3) -0.3318(4) 0.0606(16) Uani 1 1 d .
H17A H 0.1162 0.0883 -0.3610 0.091 Uiso 1 1 calc R
H17B H 0.2640 0.1238 -0.3440 0.091 Uiso 1 1 calc R
H17C H 0.1103 0.1560 -0.3671 0.091 Uiso 1 1 calc R
C18 C 0.5062(5) 0.1127(3) 0.0508(4) 0.0479(14) Uani 1 1 d .
H18A H 0.5339 0.1471 0.0938 0.072 Uiso 1 1 calc R
H18B H 0.5747 0.1066 0.0097 0.072 Uiso 1 1 calc R
H18C H 0.5098 0.0802 0.0977 0.072 Uiso 1 1 calc R
C19 C 0.4299(5) 0.0952(2) 0.2894(4) 0.0314(10) Uani 1 1 d .
C20 C 0.5232(6) 0.1258(2) 0.3781(4) 0.0402(12) Uani 1 1 d .
C21 C 0.6290(5) 0.0947(3) 0.4580(4) 0.0470(14) Uani 1 1 d .
H21 H 0.6906 0.1145 0.5176 0.056 Uiso 1 1 calc R
C22 C 0.6456(6) 0.0358(3) 0.4519(4) 0.0471(14) Uani 1 1 d .
C23 C 0.5534(6) 0.0068(2) 0.3634(4) 0.0467(14) Uani 1 1 d .
H23 H 0.5634 -0.0331 0.3584 0.056 Uiso 1 1 calc R
C24 C 0.4452(5) 0.0357(2) 0.2809(4) 0.0378(11) Uani 1 1 d .
C25 C 0.5174(7) 0.1902(2) 0.3929(5) 0.0650(18) Uani 1 1 d .
H25A H 0.5235 0.2094 0.3285 0.098 Uiso 1 1 calc R
H25B H 0.6001 0.2019 0.4537 0.098 Uiso 1 1 calc R
H25C H 0.4251 0.2003 0.4060 0.098 Uiso 1 1 calc R
C26 C 0.7648(7) 0.0040(3) 0.5387(5) 0.075(2) Uani 1 1 d .
H26A H 0.7278 -0.0333 0.5505 0.113 Uiso 1 1 calc R
H26B H 0.7901 0.0258 0.6049 0.113 Uiso 1 1 calc R
H26C H 0.8524 -0.0006 0.5156 0.113 Uiso 1 1 calc R
C27 C 0.3528(6) -0.0002(2) 0.1867(5) 0.0526(14) Uani 1 1 d .
H27A H 0.4134 -0.0308 0.1723 0.079 Uiso 1 1 calc R
H27B H 0.3172 0.0238 0.1235 0.079 Uiso 1 1 calc R
H27C H 0.2690 -0.0165 0.2046 0.079 Uiso 1 1 calc R
Cl1 Cl 0.34091(14) 0.26259(5) 0.11981(10) 0.0431(3) Uani 1 1 d .
Cl2 Cl 0.10174(17) 0.33766(6) 0.21529(12) 0.0541(4) Uani 1 1 d .
N1 N 0.0497(5) 0.21358(17) 0.3189(3) 0.0396(10) Uani 1 1 d .
Pd1 Pd 0.17987(4) 0.239762(15) 0.21736(3) 0.03015(11) Uani 1 1 d .
Sb1 Sb 0.24464(3) 0.139596(12) 0.17878(2) 0.02630(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'
N N 0.0061 0.0033 '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'
Sb Sb -0.5866 1.5461 '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
C6 C1 C2 119.8(4)
C6 C1 Sb1 122.7(3)
C2 C1 Sb1 117.3(3)
C3 C2 C1 117.8(4)
C3 C2 C7 119.0(4)
C1 C2 C7 123.2(4)
C4 C3 C2 121.5(5)
C5 C4 C3 120.2(5)
C4 C5 C6 119.4(5)
C5 C6 C1 121.2(5)
N1 C7 C2 116.5(4)
C15 C10 C11 120.4(4)
C15 C10 Sb1 122.8(3)
C11 C10 Sb1 116.4(3)
C12 C11 C10 118.1(4)
C12 C11 C16 116.8(4)
C10 C11 C16 125.1(4)
C13 C12 C11 122.7(5)
C12 C13 C14 117.9(4)
C12 C13 C17 121.0(5)
C14 C13 C17 121.0(5)
C13 C14 C15 121.9(4)
C14 C15 C10 118.8(4)
C14 C15 C18 118.7(4)
C10 C15 C18 122.4(4)
C24 C19 C20 120.7(4)
C24 C19 Sb1 120.2(4)
C20 C19 Sb1 118.6(3)
C21 C20 C19 118.0(5)
C21 C20 C25 117.5(5)
C19 C20 C25 124.5(4)
C22 C21 C20 122.4(5)
C21 C22 C23 118.4(5)
C21 C22 C26 120.6(6)
C23 C22 C26 121.0(6)
C22 C23 C24 121.7(5)
C19 C24 C23 118.8(5)
C19 C24 C27 124.1(4)
C23 C24 C27 117.1(5)
C9 N1 C8 108.4(4)
C9 N1 C7 105.3(4)
C8 N1 C7 109.0(4)
C9 N1 Pd1 106.5(3)
C8 N1 Pd1 110.2(3)
C7 N1 Pd1 117.0(3)
N1 Pd1 Cl1 173.96(12)
N1 Pd1 Cl2 92.60(11)
Cl1 Pd1 Cl2 91.51(5)
N1 Pd1 Sb1 94.55(11)
Cl1 Pd1 Sb1 82.12(3)
Cl2 Pd1 Sb1 168.34(4)
C1 Sb1 C10 103.64(17)
C1 Sb1 C19 100.23(17)
C10 Sb1 C19 115.40(16)
C1 Sb1 Pd1 103.49(12)
C10 Sb1 Pd1 110.42(11)
C19 Sb1 Pd1 120.68(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C6 1.382(6)
C1 C2 1.395(6)
C1 Sb1 2.131(4)
C2 C3 1.386(7)
C2 C7 1.509(7)
C3 C4 1.379(7)
C4 C5 1.360(7)
C5 C6 1.374(7)
C7 N1 1.508(6)
C8 N1 1.497(7)
C9 N1 1.484(6)
C10 C15 1.401(6)
C10 C11 1.403(6)
C10 Sb1 2.133(4)
C11 C12 1.388(7)
C11 C16 1.501(6)
C12 C13 1.383(7)
C13 C14 1.385(7)
C13 C17 1.504(7)
C14 C15 1.392(6)
C15 C18 1.509(6)
C19 C24 1.389(7)
C19 C20 1.404(7)
C19 Sb1 2.147(4)
C20 C21 1.396(7)
C20 C25 1.503(7)
C21 C22 1.375(8)
C22 C23 1.381(8)
C22 C26 1.511(7)
C23 C24 1.399(7)
C24 C27 1.511(7)
Cl1 Pd1 2.3029(13)
Cl2 Pd1 2.3769(13)
N1 Pd1 2.133(4)
Pd1 Sb1 2.4831(5)
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
C6 C1 C2 C3 0.9(7)
Sb1 C1 C2 C3 176.5(3)
C6 C1 C2 C7 179.2(4)
Sb1 C1 C2 C7 -5.2(6)
C1 C2 C3 C4 1.0(7)
C7 C2 C3 C4 -177.4(5)
C2 C3 C4 C5 -1.6(8)
C3 C4 C5 C6 0.4(8)
C4 C5 C6 C1 1.5(8)
C2 C1 C6 C5 -2.1(7)
Sb1 C1 C6 C5 -177.5(4)
C3 C2 C7 N1 -110.1(5)
C1 C2 C7 N1 71.6(6)
C15 C10 C11 C12 4.3(7)
Sb1 C10 C11 C12 177.6(3)
C15 C10 C11 C16 -171.8(4)
Sb1 C10 C11 C16 1.5(6)
C10 C11 C12 C13 -2.3(7)
C16 C11 C12 C13 174.1(5)
C11 C12 C13 C14 -0.4(7)
C11 C12 C13 C17 -179.4(5)
C12 C13 C14 C15 1.2(7)
C17 C13 C14 C15 -179.8(5)
C13 C14 C15 C10 0.8(7)
C13 C14 C15 C18 -176.3(5)
C11 C10 C15 C14 -3.6(7)
Sb1 C10 C15 C14 -176.5(3)
C11 C10 C15 C18 173.4(4)
Sb1 C10 C15 C18 0.5(6)
C24 C19 C20 C21 -1.4(7)
Sb1 C19 C20 C21 170.6(4)
C24 C19 C20 C25 178.5(5)
Sb1 C19 C20 C25 -9.5(7)
C19 C20 C21 C22 0.8(8)
C25 C20 C21 C22 -179.0(5)
C20 C21 C22 C23 -0.2(8)
C20 C21 C22 C26 178.1(5)
C21 C22 C23 C24 0.1(7)
C26 C22 C23 C24 -178.2(5)
C20 C19 C24 C23 1.3(7)
Sb1 C19 C24 C23 -170.5(3)
C20 C19 C24 C27 -178.1(5)
Sb1 C19 C24 C27 10.1(6)
C22 C23 C24 C19 -0.6(7)
C22 C23 C24 C27 178.8(5)
C2 C7 N1 C9 169.0(4)
C2 C7 N1 C8 52.9(6)
C2 C7 N1 Pd1 -72.9(5)
C9 N1 Pd1 Cl2 -55.3(3)
C8 N1 Pd1 Cl2 62.1(3)
C7 N1 Pd1 Cl2 -172.8(3)
C9 N1 Pd1 Sb1 133.9(3)
C8 N1 Pd1 Sb1 -108.7(3)
C7 N1 Pd1 Sb1 16.5(3)
C6 C1 Sb1 C10 22.6(4)
C2 C1 Sb1 C10 -152.9(3)
C6 C1 Sb1 C19 -96.9(4)
C2 C1 Sb1 C19 87.6(4)
C6 C1 Sb1 Pd1 137.9(4)
C2 C1 Sb1 Pd1 -37.6(4)
C15 C10 Sb1 C1 -135.4(4)
C11 C10 Sb1 C1 51.5(4)
C15 C10 Sb1 C19 -26.8(4)
C11 C10 Sb1 C19 160.0(3)
C15 C10 Sb1 Pd1 114.4(3)
C11 C10 Sb1 Pd1 -58.7(3)
C24 C19 Sb1 C1 52.9(4)
C20 C19 Sb1 C1 -119.1(4)
C24 C19 Sb1 C10 -57.7(4)
C20 C19 Sb1 C10 130.3(4)
C24 C19 Sb1 Pd1 165.4(3)
C20 C19 Sb1 Pd1 -6.6(4)
N1 Pd1 Sb1 C1 26.68(17)
Cl1 Pd1 Sb1 C1 -158.39(13)
Cl2 Pd1 Sb1 C1 -101.0(2)
N1 Pd1 Sb1 C10 137.05(17)
Cl1 Pd1 Sb1 C10 -48.02(13)
Cl2 Pd1 Sb1 C10 9.4(2)
N1 Pd1 Sb1 C19 -84.09(18)
Cl1 Pd1 Sb1 C19 90.84(14)
Cl2 Pd1 Sb1 C19 148.2(2)
