#------------------------------------------------------------------------------
#$Date: 2017-08-07 04:53:34 +0300 (Mon, 07 Aug 2017) $
#$Revision: 199607 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/88/2008879.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2008879
loop_
_publ_author_name
'Hubin, Timothy J.'
'Alcock, Nathaniel W.'
'Busch, Daryle H.'
_publ_section_title
;
 The square-pyramidal PdII complex of a cross-bridged
 tetraazamacrocycle
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1404
_journal_page_last               1406
_journal_paper_doi               10.1107/S0108270199007817
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[PdCl(C14 H30 N4 )]Cl , 2H2 0'
_chemical_formula_moiety         '[PdCl(C14 H30 N4 )]Cl , 2H2 0'
_chemical_formula_sum            'C14 H34 Cl2 N4 O2 Pd'
_chemical_formula_weight         467.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.3920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.7207(13)
_cell_length_b                   7.7934(3)
_cell_length_c                   17.2154(7)
_cell_measurement_reflns_used    5706
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3894.6(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      188(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measurement_device_type
' Siemens SMART diffractometer with Cryostream cooler (Cosier & Glazer, 1986)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11454
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.945
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0420P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0888
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                3177
_reflns_number_total             4583
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            cf1310.cif
_cod_data_source_block           timpd4
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-08-07


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.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

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

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.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (5
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0420P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2008879
_cod_database_fobs_code          2008879
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
_atom_site_attached_hydrogens
Pd1 0.149785(9) 0.76690(3) 0.074625(15) 0.02182(9) Uani d . 1 . Pd 0
Cl1 0.22391(4) 0.88515(13) 0.10093(6) 0.0419(3) Uani d . 1 . Cl 0
Cl2 0.07181(4) 0.17421(12) 0.19694(6) 0.0401(3) Uani d . 1 . Cl 0
O3 0.0000 0.9380(4) 0.2500 0.0363(9) Uani d S 1 . O 2
O4 0.0000 0.4105(5) 0.2500 0.0530(12) Uani d S 1 . O 2
O5 0.04677(10) 0.6742(4) 0.34822(16) 0.0507(8) Uani d . 1 . O 2
N1 0.08064(10) 0.6920(4) 0.06635(17) 0.0253(7) Uani d . 1 . N 0
C2 0.07598(14) 0.7027(5) 0.1516(2) 0.0344(9) Uani d . 1 . C 0
H2A 0.0756 0.8244 0.1679 0.041 Uiso calc R 1 . H 0
H2B 0.0466 0.6491 0.1572 0.041 Uiso calc R 1 . H 0
C3 0.11567(13) 0.6118(5) 0.2039(2) 0.0326(9) Uani d . 1 . C 0
H3A 0.1134 0.6220 0.2603 0.039 Uiso calc R 1 . H 0
H3B 0.1150 0.4884 0.1899 0.039 Uiso calc R 1 . H 0
N4 0.15940(11) 0.6903(4) 0.19263(17) 0.0265(7) Uani d . 1 . N 0
C5 0.19811(14) 0.5646(5) 0.2152(2) 0.0371(10) Uani d . 1 . C 0
H5A 0.2033 0.5456 0.2733 0.045 Uiso calc R 1 . H 0
H5B 0.2263 0.6190 0.2046 0.045 Uiso calc R 1 . H 0
C6 0.19290(14) 0.3896(5) 0.1748(2) 0.0361(10) Uani d . 1 . C 0
H6A 0.2178 0.3147 0.2040 0.043 Uiso calc R 1 . H 0
H6B 0.1633 0.3397 0.1814 0.043 Uiso calc R 1 . H 0
C7 0.19395(14) 0.3808(5) 0.0871(2) 0.0364(10) Uani d . 1 . C 0
H7A 0.2227 0.4353 0.0790 0.044 Uiso calc R 1 . H 0
H7B 0.1947 0.2588 0.0713 0.044 Uiso calc R 1 . H 0
N8 0.15439(10) 0.4652(4) 0.03486(17) 0.0258(7) Uani d . 1 . N 0
C9 0.16265(15) 0.4978(5) -0.0449(2) 0.0376(10) Uani d . 1 . C 0
H9A 0.1582 0.3899 -0.0760 0.045 Uiso calc R 1 . H 0
H9B 0.1950 0.5349 -0.0403 0.045 Uiso calc R 1 . H 0
C10 0.13058(15) 0.6347(5) -0.0890(2) 0.0361(10) Uani d . 1 . C 0
H10A 0.1358 0.6457 -0.1436 0.043 Uiso calc R 1 . H 0
H10B 0.0983 0.5979 -0.0930 0.043 Uiso calc R 1 . H 0
N11 0.13749(11) 0.8070(4) -0.04880(17) 0.0288(7) Uani d . 1 . N 0
C12 0.09649(15) 0.9184(5) -0.0771(2) 0.0417(11) Uani d . 1 . C 0
H12A 0.0934 0.9384 -0.1348 0.050 Uiso calc R 1 . H 0
H12B 0.1024 1.0310 -0.0502 0.050 Uiso calc R 1 . H 0
C13 0.05087(16) 0.8498(6) -0.0637(2) 0.0468(12) Uani d . 1 . C 0
H13A 0.0445 0.7395 -0.0924 0.056 Uiso calc R 1 . H 0
H13B 0.0263 0.9310 -0.0881 0.056 Uiso calc R 1 . H 0
C14 0.04746(15) 0.8209(5) 0.0222(2) 0.0406(10) Uani d . 1 . C 0
H14A 0.0526 0.9318 0.0508 0.049 Uiso calc R 1 . H 0
H14B 0.0158 0.7830 0.0229 0.049 Uiso calc R 1 . H 0
C15 0.06985(13) 0.5147(4) 0.0338(2) 0.0316(9) Uani d . 1 . C 0
H15A 0.0533 0.5262 -0.0223 0.038 Uiso calc R 1 . H 0
H15B 0.0482 0.4618 0.0632 0.038 Uiso calc R 1 . H 0
C16 0.10970(13) 0.3886(4) 0.0361(2) 0.0296(9) Uani d . 1 . C 0
H16A 0.1130 0.3181 0.0849 0.036 Uiso calc R 1 . H 0
H16B 0.1013 0.3103 -0.0100 0.036 Uiso calc R 1 . H 0
C17 0.17008(15) 0.8418(5) 0.2463(2) 0.0373(10) Uani d . 1 . C 0
H17A 0.1746 0.8042 0.3018 0.056 Uiso calc R 1 . H 0
H17B 0.1444 0.9233 0.2346 0.056 Uiso calc R 1 . H 0
H17C 0.1982 0.8974 0.2378 0.056 Uiso calc R 1 . H 0
C18 0.17671(16) 0.8951(5) -0.0750(3) 0.0486(12) Uani d . 1 . C 0
H18A 0.1691 0.9096 -0.1329 0.073 Uiso calc R 1 . H 0
H18B 0.2047 0.8254 -0.0597 0.073 Uiso calc R 1 . H 0
H18C 0.1819 1.0079 -0.0494 0.073 Uiso calc R 1 . H 0
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_publ_flag
N4 Pd1 N11 171.65(11) y
N4 Pd1 N1 85.07(11) y
N11 Pd1 N1 91.00(12) y
N4 Pd1 Cl1 89.87(9) y
N11 Pd1 Cl1 95.12(9) y
N1 Pd1 Cl1 169.68(8) y
N4 Pd1 N8 89.61(10) y
N11 Pd1 N8 82.45(10) y
N1 Pd1 N8 80.12(10) y
Cl1 Pd1 N8 108.89(7) y
C14 N1 C15 111.4(3) ?
C14 N1 C2 105.6(3) ?
C15 N1 C2 111.0(3) ?
C14 N1 Pd1 112.0(2) ?
C15 N1 Pd1 114.0(2) ?
C2 N1 Pd1 102.2(2) ?
C3 C2 N1 109.5(3) ?
N4 C3 C2 108.9(3) ?
C3 N4 C17 108.7(3) ?
C3 N4 C5 110.0(3) ?
C17 N4 C5 107.9(3) ?
C3 N4 Pd1 107.8(2) ?
C17 N4 Pd1 110.2(2) ?
C5 N4 Pd1 112.3(2) ?
N4 C5 C6 118.0(3) ?
C7 C6 C5 118.2(3) ?
N8 C7 C6 113.7(3) ?
C16 N8 C9 114.8(3) ?
C16 N8 C7 114.7(3) ?
C9 N8 C7 112.1(3) ?
C16 N8 Pd1 106.32(19) ?
C9 N8 Pd1 97.20(19) ?
C7 N8 Pd1 110.0(2) ?
N8 C9 C10 112.0(3) ?
N11 C10 C9 112.8(3) ?
C12 N11 C18 105.5(3) ?
C12 N11 C10 110.4(3) ?
C18 N11 C10 108.0(3) ?
C12 N11 Pd1 111.7(2) ?
C18 N11 Pd1 113.2(3) ?
C10 N11 Pd1 108.0(2) ?
N11 C12 C13 116.0(3) ?
C12 C13 C14 116.6(4) ?
N1 C14 C13 114.8(3) ?
N1 C15 C16 118.6(3) ?
N8 C16 C15 116.0(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N4 . 2.078(3) y
Pd1 N11 . 2.101(3) y
Pd1 N1 . 2.112(3) y
Pd1 Cl1 . 2.3407(10) y
Pd1 N8 . 2.461(3) y
N1 C14 . 1.496(5) ?
N1 C15 . 1.499(4) ?
N1 C2 . 1.506(4) ?
C2 C3 . 1.500(5) ?
C3 N4 . 1.487(5) ?
N4 C17 . 1.491(5) ?
N4 C5 . 1.497(5) ?
C5 C6 . 1.524(5) ?
C6 C7 . 1.519(5) ?
C7 N8 . 1.473(5) ?
N8 C16 . 1.460(4) ?
N8 C9 . 1.468(4) ?
C9 C10 . 1.521(5) ?
C10 N11 . 1.504(5) ?
N11 C12 . 1.491(5) ?
N11 C18 . 1.503(5) ?
C12 C13 . 1.521(6) ?
C13 C14 . 1.521(5) ?
C15 C16 . 1.533(5) ?
