#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/18/8101820.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_8101820
loop_
_publ_author_name
'G.-F. Zhang'
'Y.-L. Dou'
'X.-Z. Fan'
_publ_section_title
;
Crystal structure of dichloro[1,3-bis(5-methyl-3-phenylpyrazol-1-yl)
propan-2-ol]palladium(II), Pd[(C₁₀H₉N₂)₂C₃H₅OH]Cl₂
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              451
_journal_page_last               452
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety         'C23 H24 Cl2 N4 O Pd'
_chemical_formula_sum            'C23 H24 Cl2 N4 O Pd'
_chemical_formula_weight         549.76
_chemical_name_systematic
; 
 dichloro[1,3-bis(5-methyl-3-phenylpyrazol-1-yl)propan-2-ol]palladium(II) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.08(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8868(18)
_cell_length_b                   16.192(3)
_cell_length_c                   16.228(3)
_cell_measurement_reflns_used    6223
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      2.63
_cell_volume                     2317.3(8)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       phi/omega
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17640
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0409P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                4764
_reflns_number_total             6223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1586.cff
_cod_data_source_block           dl-1
_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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P12(1)/c1
_cod_database_code               8101820
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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.636506(16) 0.931772(10) 0.160631(10) 0.02948(6) Uani 1 4 e d . . .
C1 C 0.7002(4) 0.8621(2) 0.51269(19) 0.0829(11) Uani 1 4 e d . . .
H1A H 0.6822 0.8345 0.5607 0.099 Uiso 1 4 e calc R . .
C2 C 0.2460(3) 0.67535(19) 0.1035(2) 0.0749(10) Uani 1 4 e d . . .
H2A H 0.1922 0.7113 0.0630 0.112 Uiso 1 4 e calc R . .
H2B H 0.1832 0.6631 0.1460 0.112 Uiso 1 4 e calc R . .
H2C H 0.2712 0.6250 0.0771 0.112 Uiso 1 4 e calc R . .
C3 C 0.5814(3) 0.8803(2) 0.45236(18) 0.0675(9) Uani 1 4 e d . . .
H3A H 0.4835 0.8643 0.4597 0.081 Uiso 1 4 e calc R . .
C4 C 0.8718(3) 0.92437(19) 0.4308(2) 0.0627(8) Uani 1 4 e d . . .
H4A H 0.9706 0.9386 0.4234 0.075 Uiso 1 4 e calc R . .
C5 C 0.0820(3) 1.0108(2) 0.2490(2) 0.0656(9) Uani 1 4 e d . . .
H5A H 0.0548 1.0189 0.1905 0.098 Uiso 1 4 e calc R . .
H5B H 0.0701 1.0618 0.2777 0.098 Uiso 1 4 e calc R . .
H5C H 0.0175 0.9695 0.2685 0.098 Uiso 1 4 e calc R . .
C6 C 0.8440(4) 0.8846(2) 0.5016(2) 0.0734(10) Uani 1 4 e d . . .
H6A H 0.9239 0.8728 0.5426 0.088 Uiso 1 4 e calc R . .
C7 C 0.3650(3) 0.84386(16) 0.04884(15) 0.0437(6) Uani 1 4 e d . . .
H7A H 0.3209 0.8080 0.0044 0.052 Uiso 1 4 e calc R . .
H7B H 0.4453 0.8750 0.0278 0.052 Uiso 1 4 e calc R . .
C8 C 0.7600(3) 0.74658(14) 0.26308(15) 0.0411(5) Uani 1 4 e d . . .
C9 C 1.0390(3) 0.7337(2) 0.3584(2) 0.0663(8) Uani 1 4 e d . . .
H9A H 1.1327 0.7291 0.3906 0.080 Uiso 1 4 e calc R . .
C10 C 1.0307(3) 0.76480(19) 0.28058(19) 0.0586(7) Uani 1 4 e d . . .
H10A H 1.1182 0.7817 0.2593 0.070 Uiso 1 4 e calc R . .
C11 C 0.9107(4) 0.70910(19) 0.39005(19) 0.0683(8) Uani 1 4 e d . . .
H11A H 0.9179 0.6885 0.4439 0.082 Uiso 1 4 e calc R . .
C12 C 0.8906(3) 0.77127(16) 0.23280(16) 0.0490(6) Uani 1 4 e d . . .
H12A H 0.8849 0.7927 0.1793 0.059 Uiso 1 4 e calc R . .
C13 C 0.3883(3) 0.71688(15) 0.14151(18) 0.0502(6) Uani 1 4 e d . . .
C14 C 0.2447(2) 0.98304(16) 0.26522(16) 0.0445(6) Uani 1 4 e d . . .
C15 C 0.3297(3) 0.96478(18) 0.33884(16) 0.0486(6) Uani 1 4 e d . . .
H15A H 0.2973 0.9654 0.3912 0.058 Uiso 1 4 e calc R . .
C16 C 0.4988(3) 0.68939(15) 0.20112(18) 0.0526(7) Uani 1 4 e d . . .
H16A H 0.4985 0.6398 0.2300 0.063 Uiso 1 4 e calc R . .
C17 C 0.2427(2) 0.90485(16) 0.06847(17) 0.0443(6) Uani 1 4 e d . . .
H17A H 0.1887 0.9226 0.0151 0.053 Uiso 1 4 e calc R . .
C18 C 0.7698(3) 0.71449(17) 0.34282(18) 0.0571(7) Uani 1 4 e d . . .
H18A H 0.6831 0.6968 0.3644 0.068 Uiso 1 4 e calc R . .
C19 C 0.4747(2) 0.94497(14) 0.32032(15) 0.0389(5) Uani 1 4 e d . . .
C21 C 0.7538(3) 0.94358(16) 0.37012(17) 0.0484(6) Uani 1 4 e d . . .
H21A H 0.7733 0.9707 0.3221 0.058 Uiso 1 4 e calc R . .
C22 C 0.2952(3) 0.98329(14) 0.11587(15) 0.0411(5) Uani 1 4 e d . . .
H22A H 0.3826 1.0049 0.0926 0.049 Uiso 1 4 e calc R . .
H22B H 0.2151 1.0241 0.1062 0.049 Uiso 1 4 e calc R . .
C23 C 0.6117(2) 0.74930(14) 0.21057(15) 0.0381(5) Uani 1 4 e d . . .
C20 C 0.6066(3) 0.92242(14) 0.38083(15) 0.0408(5) Uani 1 4 e d . . .
N1 N 0.47803(18) 0.95082(11) 0.23864(12) 0.0335(4) Uani 1 4 e d . . .
N2 N 0.33517(18) 0.97430(12) 0.20488(12) 0.0374(4) Uani 1 4 e d . . .
N3 N 0.43340(19) 0.79197(11) 0.11677(12) 0.0391(4) Uani 1 4 e d . . .
N4 N 0.57186(19) 0.81202(11) 0.15891(11) 0.0336(4) Uani 1 4 e d . . .
O1 O 0.13877(19) 0.86010(12) 0.10903(13) 0.0661(6) Uani 1 4 e d . . .
H1B H 0.0715 0.8911 0.1207 0.099 Uiso 1 4 e calc R . .
Cl1 Cl 0.69491(8) 1.06876(4) 0.16294(5) 0.05172(16) Uani 1 4 e d . . .
Cl2 Cl 0.79483(7) 0.90881(4) 0.06195(4) 0.04650(15) Uani 1 4 e 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'
O O 0.0106 0.0060 '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
N4 Pd1 N1 86.36(7) . . ?
N4 Pd1 Cl1 176.65(5) . . ?
N1 Pd1 Cl1 90.92(5) . . ?
N4 Pd1 Cl2 91.87(5) . . ?
N1 Pd1 Cl2 174.08(5) . . ?
Cl1 Pd1 Cl2 90.64(3) . . ?
C6 C1 C3 119.8(3) . . ?
C6 C1 H1A 120.1 . . ?
C3 C1 H1A 120.1 . . ?
C13 C2 H2A 109.5 . . ?
C13 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C13 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 C20 120.7(3) . . ?
C1 C3 H3A 119.7 . . ?
C20 C3 H3A 119.7 . . ?
C6 C4 C21 120.4(3) . . ?
C6 C4 H4A 119.8 . . ?
C21 C4 H4A 119.8 . . ?
C14 C5 H5A 109.5 . . ?
C14 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C14 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C1 C6 C4 120.5(3) . . ?
C1 C6 H6A 119.8 . . ?
C4 C6 H6A 119.8 . . ?
N3 C7 C17 117.1(2) . . ?
N3 C7 H7A 108.0 . . ?
C17 C7 H7A 108.0 . . ?
N3 C7 H7B 108.0 . . ?
C17 C7 H7B 108.0 . . ?
H7A C7 H7B 107.3 . . ?
C12 C8 C18 118.9(2) . . ?
C12 C8 C23 121.1(2) . . ?
C18 C8 C23 119.8(2) . . ?
C10 C9 C11 120.5(3) . . ?
C10 C9 H9A 119.8 . . ?
C11 C9 H9A 119.8 . . ?
C9 C10 C12 119.5(3) . . ?
C9 C10 H10A 120.3 . . ?
C12 C10 H10A 120.3 . . ?
C9 C11 C18 120.8(3) . . ?
C9 C11 H11A 119.6 . . ?
C18 C11 H11A 119.6 . . ?
C8 C12 C10 121.2(3) . . ?
C8 C12 H12A 119.4 . . ?
C10 C12 H12A 119.4 . . ?
N3 C13 C16 106.8(2) . . ?
N3 C13 C2 123.1(2) . . ?
C16 C13 C2 130.0(2) . . ?
N2 C14 C15 107.3(2) . . ?
N2 C14 C5 123.4(2) . . ?
C15 C14 C5 129.3(2) . . ?
C14 C15 C19 106.7(2) . . ?
C14 C15 H15A 126.7 . . ?
C19 C15 H15A 126.7 . . ?
C13 C16 C23 107.3(2) . . ?
C13 C16 H16A 126.4 . . ?
C23 C16 H16A 126.4 . . ?
O1 C17 C22 111.8(2) . . ?
O1 C17 C7 106.9(2) . . ?
C22 C17 C7 117.45(19) . . ?
O1 C17 H17A 106.7 . . ?
C22 C17 H17A 106.7 . . ?
C7 C17 H17A 106.7 . . ?
C11 C18 C8 119.2(3) . . ?
C11 C18 H18A 120.4 . . ?
C8 C18 H18A 120.4 . . ?
N1 C19 C15 109.4(2) . . ?
N1 C19 C20 124.4(2) . . ?
C15 C19 C20 126.2(2) . . ?
C20 C21 C4 120.0(3) . . ?
C20 C21 H21A 120.0 . . ?
C4 C21 H21A 120.0 . . ?
N2 C22 C17 116.1(2) . . ?
N2 C22 H22A 108.3 . . ?
C17 C22 H22A 108.3 . . ?
N2 C22 H22B 108.3 . . ?
C17 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
N4 C23 C16 109.2(2) . . ?
N4 C23 C8 122.1(2) . . ?
C16 C23 C8 128.5(2) . . ?
C21 C20 C3 118.6(2) . . ?
C21 C20 C19 122.7(2) . . ?
C3 C20 C19 118.7(2) . . ?
C19 N1 N2 106.48(17) . . ?
C19 N1 Pd1 135.36(14) . . ?
N2 N1 Pd1 118.15(14) . . ?
C14 N2 N1 110.13(19) . . ?
C14 N2 C22 128.10(18) . . ?
N1 N2 C22 121.72(18) . . ?
C13 N3 N4 110.14(19) . . ?
C13 N3 C7 129.0(2) . . ?
N4 N3 C7 120.38(18) . . ?
C23 N4 N3 106.55(17) . . ?
C23 N4 Pd1 131.87(15) . . ?
N3 N4 Pd1 118.04(13) . . ?
C17 O1 H1B 109.5 . . ?
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
Pd1 N4 2.0215(18) . ?
Pd1 N1 2.0299(18) . ?
Pd1 Cl1 2.2773(7) . ?
Pd1 Cl2 2.2886(8) . ?
C1 C6 1.362(4) . ?
C1 C3 1.380(4) . ?
C1 H1A 0.9300 . ?
C2 C13 1.497(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C20 1.388(4) . ?
C3 H3A 0.9300 . ?
C4 C6 1.366(4) . ?
C4 C21 1.383(4) . ?
C4 H4A 0.9300 . ?
C5 C14 1.506(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9300 . ?
C7 N3 1.458(3) . ?
C7 C17 1.531(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C12 1.374(3) . ?
C8 C18 1.387(3) . ?
C8 C23 1.479(3) . ?
C9 C10 1.353(4) . ?
C9 C11 1.366(4) . ?
C9 H9A 0.9300 . ?
C10 C12 1.387(3) . ?
C10 H10A 0.9300 . ?
C11 C18 1.388(4) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 N3 1.356(3) . ?
C13 C16 1.365(4) . ?
C14 N2 1.349(3) . ?
C14 C15 1.365(3) . ?
C15 C19 1.396(3) . ?
C15 H15A 0.9300 . ?
C16 C23 1.391(3) . ?
C16 H16A 0.9300 . ?
C17 O1 1.401(3) . ?
C17 C22 1.528(3) . ?
C17 H17A 0.9800 . ?
C18 H18A 0.9300 . ?
C19 N1 1.333(3) . ?
C19 C20 1.479(3) . ?
C21 C20 1.384(3) . ?
C21 H21A 0.9300 . ?
C22 N2 1.452(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 N4 1.337(3) . ?
N1 N2 1.373(2) . ?
N3 N4 1.371(2) . ?
O1 H1B 0.8200 . ?
