#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:01:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179499 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/96/4339652.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_4339652
loop_
_publ_author_name
'Walmsley, Judith A.'
'Zhu, Shourong'
'Matilla, Antonio'
'Donowick, Tiffanee G.'
'Cramp, Jessica E.'
'Tercero, Jose Manuel'
'Dalrymple, Tatyana'
_publ_section_title
;
 Cyclic tetranuclear and hexanuclear palladium(II) complexes and their
 host-guest chemistry.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9945
_journal_page_last               9953
_journal_paper_doi               10.1021/ic700830v
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C3 H10 Cl2 N2 O Pd'
_chemical_formula_sum            'C3 H10 Cl2 N2 O Pd'
_chemical_formula_weight         267.43
_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
_audit_update_record
;
2007-02-05 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.533(2)
_cell_length_b                   8.766(2)
_cell_length_c                   10.749(2)
_cell_measurement_temperature    293(2)
_cell_volume                     776.6(3)
_computing_cell_refinement       'DIF4 Control program vers. 7 (STOE & CIE)'
_computing_data_collection       'DIF4 Control program vers. 7 (STOE & CIE)'
_computing_data_reduction        'DIF4 Control program vers. 7 (STOE & CIE)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe-Siemens AED 2'
_diffrn_measurement_method       'omega / 2theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5586
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    3.002
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.674
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         2818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0312
_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)+(0.0189P)²+0.1090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0593
_reflns_number_gt                2155
_reflns_number_total             2818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700830v-file003.cif
_cod_data_source_block           dulce
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/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               4339652
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
Pd1 Pd 1.11612(2) -0.07894(2) 0.842796(19) 0.02585(6) Uani 1 1 d .
N1 N 1.1448(3) 0.1478(3) 0.8127(2) 0.0331(5) Uani 1 1 d .
H1A H 1.2125 0.1868 0.8841 0.040 Uiso 1 1 calc R
H1B H 1.1935 0.1575 0.7482 0.040 Uiso 1 1 calc R
C2 C 0.9951(4) 0.2411(3) 0.7807(3) 0.0340(6) Uani 1 1 d .
H2A H 1.0237 0.3466 0.7706 0.041 Uiso 1 1 calc R
H2B H 0.9446 0.2363 0.8518 0.041 Uiso 1 1 calc R
C3 C 0.8740(4) 0.1890(3) 0.6589(3) 0.0308(5) Uani 1 1 d .
H3 H 0.7805 0.2579 0.6431 0.037 Uiso 1 1 calc R
O3 O 0.9419(3) 0.1978(2) 0.54991(18) 0.0381(5) Uani 1 1 d .
H3A H 0.9774 0.2867 0.5436 0.046 Uiso 1 1 d R
C4 C 0.8121(3) 0.0284(3) 0.6607(3) 0.0307(5) Uani 1 1 d .
H4A H 0.7636 0.0172 0.7324 0.037 Uiso 1 1 calc R
H4B H 0.7284 0.0098 0.5820 0.037 Uiso 1 1 calc R
N5 N 0.9425(3) -0.0864(3) 0.6726(2) 0.0293(4) Uani 1 1 d .
H5A H 0.9902 -0.0724 0.6080 0.035 Uiso 1 1 calc R
H5B H 0.8975 -0.1799 0.6632 0.035 Uiso 1 1 calc R
Cl1 Cl 1.31209(9) -0.06385(8) 1.03617(7) 0.03571(15) Uani 1 1 d .
Cl2 Cl 1.08234(10) -0.33676(9) 0.86765(7) 0.03920(16) Uani 1 1 d .
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
Pd1 0.03061(10) 0.02007(9) 0.02720(9) 0.00101(8) 0.00806(7) -0.00059(9)
N1 0.0438(13) 0.0221(12) 0.0315(11) 0.0007(9) 0.0062(10) -0.0061(11)
C2 0.0441(16) 0.0223(13) 0.0354(13) -0.0031(11) 0.0099(12) -0.0004(12)
C3 0.0379(14) 0.0239(12) 0.0317(12) -0.0014(11) 0.0112(11) 0.0017(12)
O3 0.0528(13) 0.0293(10) 0.0371(10) 0.0024(9) 0.0206(10) -0.0045(10)
C4 0.0328(13) 0.0245(12) 0.0356(13) -0.0023(11) 0.0102(11) -0.0001(12)
N5 0.0365(11) 0.0218(10) 0.0299(10) -0.0011(9) 0.0091(9) -0.0017(10)
Cl1 0.0402(3) 0.0292(3) 0.0338(3) -0.0001(3) 0.0025(3) -0.0003(3)
Cl2 0.0454(4) 0.0237(3) 0.0450(4) 0.0062(3) 0.0055(3) -0.0032(3)
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
N5 Pd1 N1 88.74(10)
N5 Pd1 Cl2 89.36(7)
N1 Pd1 Cl2 177.59(7)
N5 Pd1 Cl1 178.54(7)
N1 Pd1 Cl1 89.90(7)
Cl2 Pd1 Cl1 92.01(3)
C2 N1 Pd1 116.33(18)
C2 N1 H1A 108.2
Pd1 N1 H1A 108.2
C2 N1 H1B 108.2
Pd1 N1 H1B 108.2
H1A N1 H1B 107.4
N1 C2 C3 112.9(2)
N1 C2 H2A 109.0
C3 C2 H2A 109.0
N1 C2 H2B 109.0
C3 C2 H2B 109.0
H2A C2 H2B 107.8
O3 C3 C4 106.1(2)
O3 C3 C2 111.1(2)
C4 C3 C2 115.7(2)
O3 C3 H3 107.9
C4 C3 H3 107.9
C2 C3 H3 107.9
C3 O3 H3A 110.1
N5 C4 C3 112.2(2)
N5 C4 H4A 109.2
C3 C4 H4A 109.2
N5 C4 H4B 109.2
C3 C4 H4B 109.2
H4A C4 H4B 107.9
C4 N5 Pd1 114.30(17)
C4 N5 H5A 108.7
Pd1 N5 H5A 108.7
C4 N5 H5B 108.7
Pd1 N5 H5B 108.7
H5A N5 H5B 107.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 N5 2.035(2)
Pd1 N1 2.039(2)
Pd1 Cl2 2.3027(9)
Pd1 Cl1 2.3096(11)
N1 C2 1.481(4)
N1 H1A 0.9000
N1 H1B 0.9000
C2 C3 1.513(4)
C2 H2A 0.9700
C2 H2B 0.9700
C3 O3 1.438(3)
C3 C4 1.505(4)
C3 H3 0.9800
O3 H3A 0.8453
C4 N5 1.481(4)
C4 H4A 0.9700
C4 H4B 0.9700
N5 H5A 0.9000
N5 H5B 0.9000
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5B Cl1 0.90 2.63 3.456(3) 152.7 4
N5 H5A O3 0.90 2.22 2.978(3) 141.5 3_756
O3 H3A Cl1 0.85 2.80 3.386(2) 127.9 4_565
O3 H3A Cl1 0.85 2.55 3.261(2) 143.2 2_756
N1 H1B Cl2 0.90 2.54 3.396(3) 159.5 2_756
N1 H1A O3 0.90 2.50 3.378(4) 167.1 4_666
