#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:40:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179418 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/15/4331543.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_4331543
loop_
_publ_author_name
'Yu, Shu-Yan'
'Huang, Hai-Ping'
'Li, Sheng-Hui'
'Jiao, Qing'
'Li, Yi-Zhi'
'Wu, Biao'
'Sei, Yoshihisa'
'Yamaguchi, Kentaro'
'Pan, Yuan-Jiang'
'Ma, Hong-Wei'
_publ_section_title
;
 Solution self-assembly, spontaneous deprotonation, and crystal structures
 of bipyrazolate-bridged metallomacrocycles with dimetal centers.
;
_journal_issue                   25
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9471
_journal_page_last               9488
_journal_paper_doi               10.1021/ic0509332
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C72 H64 N16 Pd4, 8(H2 O), 4(N O3)'
_chemical_formula_sum            'C72 H80 N20 O20 Pd4'
_chemical_formula_weight         1971.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.463(4)
_cell_length_b                   20.759(4)
_cell_length_c                   22.208(4)
_cell_measurement_reflns_used    1723
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.21
_cell_volume                     8512(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8544
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Bruker, 2000)'
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.489
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0612P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                3185
_reflns_number_total             4302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0509332sup1.cif
_cod_data_source_block           15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Adding full bibliography for 4331538--4331543.cif.
;
_cod_original_sg_symbol_H-M      'Ibam '
_cod_database_code               4331543
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, 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
Pd1 Pd 0.635556(19) 0.342113(15) 0.072249(14) 0.03069(13) Uani 1 1 d . . .
N1 N 0.6211(2) 0.2548(2) 0.11117(19) 0.0443(10) Uani 1 1 d . . .
N2 N 0.7327(2) 0.33093(18) 0.11360(17) 0.0375(9) Uani 1 1 d . . .
N3 N 0.65648(18) 0.42569(16) 0.02919(15) 0.0270(7) Uani 1 1 d . . .
N4 N 0.53937(19) 0.34526(18) 0.03024(15) 0.0314(8) Uani 1 1 d . . .
N5 N 0.8752(3) 0.1162(3) 0.2565(3) 0.0663(15) Uani 1 1 d . . .
C1 C 0.5708(3) 0.2189(3) 0.1088(3) 0.0573(15) Uani 1 1 d . . .
H1 H 0.5297 0.2364 0.0910 0.069 Uiso 1 1 calc R . .
C2 C 0.5623(3) 0.1548(3) 0.1282(2) 0.0501(13) Uani 1 1 d . . .
H2 H 0.5213 0.1304 0.1197 0.060 Uiso 1 1 calc R . .
C3 C 0.6205(3) 0.1309(3) 0.1613(3) 0.0500(13) Uani 1 1 d . . .
H3 H 0.6199 0.0897 0.1777 0.060 Uiso 1 1 calc R . .
C4 C 0.6792(3) 0.1716(2) 0.1686(2) 0.0428(12) Uani 1 1 d . . .
H4 H 0.7196 0.1577 0.1899 0.051 Uiso 1 1 calc R . .
C5 C 0.6780(3) 0.2339(2) 0.1436(2) 0.0400(11) Uani 1 1 d . . .
C6 C 0.7397(3) 0.2794(2) 0.14508(19) 0.0393(11) Uani 1 1 d . . .
C7 C 0.8027(3) 0.2652(3) 0.1783(2) 0.0470(13) Uani 1 1 d . . .
H7 H 0.8068 0.2281 0.2014 0.056 Uiso 1 1 calc R . .
C8 C 0.8578(3) 0.3095(3) 0.1744(2) 0.0481(13) Uani 1 1 d . . .
H8 H 0.9008 0.3016 0.1948 0.058 Uiso 1 1 calc R . .
C9 C 0.8515(3) 0.3650(3) 0.1415(3) 0.0539(14) Uani 1 1 d . . .
H9 H 0.8890 0.3949 0.1405 0.065 Uiso 1 1 calc R . .
C10 C 0.7872(3) 0.3760(3) 0.1092(2) 0.0458(12) Uani 1 1 d . . .
H10 H 0.7816 0.4126 0.0855 0.055 Uiso 1 1 calc R . .
C11 C 0.4721(3) 0.3534(2) 0.05019(18) 0.0316(9) Uani 1 1 d . . .
C12 C 0.4528(3) 0.3550(3) 0.11602(19) 0.0465(13) Uani 1 1 d . . .
H12A H 0.4610 0.3133 0.1334 0.070 Uiso 1 1 calc R . .
H12B H 0.4028 0.3665 0.1205 0.070 Uiso 1 1 calc R . .
H12C H 0.4825 0.3863 0.1362 0.070 Uiso 1 1 calc R . .
C13 C 0.4252(4) 0.3546(3) 0.0000 0.0321(13) Uani 1 2 d S . .
C14 C 0.3459(4) 0.3539(3) 0.0000 0.0397(15) Uani 1 2 d S . .
C15 C 0.3128(4) 0.2903(3) 0.0000 0.0359(14) Uani 1 2 d S . .
H15 H 0.3423 0.2539 0.0000 0.043 Uiso 1 2 calc SR . .
C16 C 0.2372(4) 0.2827(4) 0.0000 0.0458(17) Uani 1 2 d S . .
H16 H 0.2164 0.2419 0.0000 0.055 Uiso 1 2 calc SR . .
C17 C 0.1967(4) 0.3343(3) 0.0000 0.0445(17) Uani 1 2 d S . .
H17 H 0.1467 0.3287 0.0000 0.053 Uiso 1 2 calc SR . .
C18 C 0.2232(4) 0.3964(4) 0.0000 0.0394(16) Uani 1 2 d S . .
H18 H 0.1921 0.4316 0.0000 0.047 Uiso 1 2 calc SR . .
C19 C 0.3006(3) 0.4051(3) 0.0000 0.0350(14) Uani 1 2 d S . .
C20 C 0.3231(3) 0.4715(3) 0.0000 0.0285(12) Uani 1 2 d S . .
C21 C 0.3335(2) 0.5138(2) -0.04970(19) 0.0313(9) Uani 1 1 d . . .
C22 C 0.3284(2) 0.4969(2) -0.11417(18) 0.0283(9) Uani 1 1 d . . .
H22A H 0.3306 0.5355 -0.1380 0.042 Uiso 1 1 calc R . .
H22B H 0.2834 0.4752 -0.1216 0.042 Uiso 1 1 calc R . .
H22C H 0.3679 0.4691 -0.1248 0.042 Uiso 1 1 calc R . .
O1 O 0.9173(3) 0.0731(2) 0.2606(2) 0.0717(13) Uani 1 1 d . . .
O2 O 0.8936(3) 0.1704(2) 0.2640(2) 0.0759(14) Uani 1 1 d . . .
O3 O 0.8119(2) 0.1038(2) 0.2508(2) 0.0664(12) Uani 1 1 d . . .
O1W O 0.2840(3) 1.0000 0.2500 0.0506(13) Uani 1 2 d S . .
H1WA H 0.2686 0.9663 0.2675 0.061 Uiso 0.50 1 d PR . .
H1WB H 0.2686 1.0331 0.2686 0.061 Uiso 0.50 1 d PR . .
O2W O 0.5000 1.0000 0.2500 0.0495(18) Uani 1 4 d S . .
H2WA H 0.5153 0.9663 0.2675 0.059 Uiso 0.25 1 d PR . .
H2WB H 0.5153 1.0006 0.2139 0.059 Uiso 0.25 1 d PR . .
O3W O 1.0000 0.0000 0.5000 0.0464(17) Uani 1 4 d S . .
H3WA H 1.0092 0.0000 0.5375 0.056 Uiso 0.25 1 d PR . .
H3WB H 0.9757 0.0334 0.4911 0.056 Uiso 0.25 1 d PR . .
O4W O 0.4885(2) 0.1574(2) 1.0000 0.0372(10) Uani 1 2 d S A 2
H4WD H 0.4601 0.1482 1.0288 0.045 Uiso 0.50 1 d PR A 2
H4WC H 0.5029 0.1229 0.9832 0.045 Uiso 0.50 1 d PR A 2
O5W O 0.4109(3) 0.0719(3) 0.0000 0.0517(13) Uani 1 2 d S B 1
H5WD H 0.4197 0.0824 -0.0363 0.062 Uiso 0.50 1 d PR B 1
H5WC H 0.4289 0.0998 0.0236 0.078 Uiso 0.50 1 d PR B 1
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'
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
N4 Pd1 N3 85.48(14) . .
N4 Pd1 N1 96.34(16) . .
N3 Pd1 N1 175.21(16) . .
N4 Pd1 N2 175.25(15) . .
N3 Pd1 N2 98.26(15) . .
N1 Pd1 N2 79.71(17) . .
N4 Pd1 Pd1 62.30(10) . 10
N3 Pd1 Pd1 61.72(10) . 10
N1 Pd1 Pd1 115.25(13) . 10
N2 Pd1 Pd1 116.92(12) . 10
C1 N1 C5 115.5(5) . .
C1 N1 Pd1 130.0(4) . .
C5 N1 Pd1 114.4(4) . .
C6 N2 C10 122.1(4) . .
C6 N2 Pd1 115.5(3) . .
C10 N2 Pd1 122.4(3) . .
N3 N3 C21 109.7(2) 10 9_665
N3 N3 Pd1 118.28(10) 10 .
C21 N3 Pd1 131.8(3) 9_665 .
C11 N4 N4 109.5(2) . 10
C11 N4 Pd1 132.5(3) . .
N4 N4 Pd1 117.70(10) 10 .
O2 N5 O1 120.9(6) . .
O2 N5 O3 119.7(6) . .
O1 N5 O3 118.9(6) . .
N1 C1 C2 131.6(6) . .
N1 C1 H1 114.2 . .
C2 C1 H1 114.2 . .
C3 C2 C1 114.3(6) . .
C3 C2 H2 122.9 . .
C1 C2 H2 122.9 . .
C4 C3 C2 116.7(5) . .
C4 C3 H3 121.6 . .
C2 C3 H3 121.6 . .
C3 C4 C5 120.2(5) . .
C3 C4 H4 119.9 . .
C5 C4 H4 119.9 . .
N1 C5 C4 121.2(5) . .
N1 C5 C6 114.0(4) . .
C4 C5 C6 124.5(4) . .
N2 C6 C7 122.8(5) . .
N2 C6 C5 116.3(4) . .
C7 C6 C5 120.9(4) . .
C8 C7 C6 116.0(5) . .
C8 C7 H7 122.0 . .
C6 C7 H7 122.0 . .
C9 C8 C7 122.3(5) . .
C9 C8 H8 118.8 . .
C7 C8 H8 118.8 . .
C8 C9 C10 118.7(6) . .
C8 C9 H9 120.7 . .
C10 C9 H9 120.7 . .
N2 C10 C9 118.1(5) . .
N2 C10 H10 120.9 . .
C9 C10 H10 120.9 . .
N4 C11 C13 108.2(4) . .
N4 C11 C12 123.2(4) . .
C13 C11 C12 128.5(4) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 C11 104.4(6) . 10
C11 C13 C14 127.8(3) . .
C11 C13 C14 127.8(3) 10 .
C19 C14 C15 116.9(6) . .
C19 C14 C13 127.7(7) . .
C15 C14 C13 115.4(6) . .
C16 C15 C14 121.2(7) . .
C16 C15 H15 119.4 . .
C14 C15 H15 119.4 . .
C17 C16 C15 118.6(7) . .
C17 C16 H16 120.7 . .
C15 C16 H16 120.7 . .
C16 C17 C18 124.2(8) . .
C16 C17 H17 117.9 . .
C18 C17 H17 117.9 . .
C17 C18 C19 118.0(7) . .
C17 C18 H18 121.0 . .
C19 C18 H18 121.0 . .
C14 C19 C18 121.1(7) . .
C14 C19 C20 125.0(6) . .
C18 C19 C20 114.0(6) . .
C21 C20 C21 101.7(5) 10 .
C21 C20 C19 129.0(3) 10 .
C21 C20 C19 129.0(3) . .
N3 C21 C20 109.3(4) 9_665 .
N3 C21 C22 123.8(4) 9_665 .
C20 C21 C22 126.7(4) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
H1WA O1W H1WB 109.5 . .
H2WA O2W H2WB 109.5 . .
H3WA O3W H3WB 109.5 . .
H4WD O4W H4WC 109.5 . .
H5WD O5W H5WC 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N4 2.007(3) .
Pd1 N3 2.018(3) .
Pd1 N1 2.027(4) .
Pd1 N2 2.028(4) .
Pd1 Pd1 3.2090(9) 10
N1 C1 1.191(7) .
N1 C5 1.347(6) .
N2 C6 1.284(6) .
N2 C10 1.377(7) .
N3 N3 1.296(7) 10
N3 C21 1.350(5) 9_665
N4 C11 1.330(6) .
N4 N4 1.343(7) 10
N5 O2 1.189(7) .
N5 O1 1.189(7) .
N5 O3 1.203(7) .
C1 C2 1.408(7) .
C1 H1 0.9300 .
C2 C3 1.393(7) .
C2 H2 0.9300 .
C3 C4 1.382(8) .
C3 H3 0.9300 .
C4 C5 1.407(6) .
C4 H4 0.9300 .
C5 C6 1.480(8) .
C6 C7 1.409(7) .
C7 C8 1.374(8) .
C7 H7 0.9300 .
C8 C9 1.369(8) .
C8 H8 0.9300 .
C9 C10 1.406(7) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C13 1.411(5) .
C11 C12 1.505(5) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C11 1.411(5) 10
C13 C14 1.464(9) .
C14 C19 1.353(9) .
C14 C15 1.455(9) .
C15 C16 1.406(10) .
C15 H15 0.9300 .
C16 C17 1.305(10) .
C16 H16 0.9300 .
C17 C18 1.380(9) .
C17 H17 0.9300 .
C18 C19 1.440(9) .
C18 H18 0.9300 .
C19 C20 1.440(9) .
C20 C21 1.423(6) 10
C20 C21 1.423(6) .
C21 N3 1.350(5) 9_665
C21 C22 1.477(6) .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
O1W H1WA 0.8500 .
O1W H1WB 0.8500 .
O2W H2WA 0.8500 .
O2W H2WB 0.8500 .
O3W H3WA 0.8500 .
O3W H3WB 0.8500 .
O4W H4WD 0.8500 .
O4W H4WC 0.8501 .
O5W H5WD 0.8500 .
O5W H5WC 0.8500 .
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
O1W H1WA O3 0.85 2.11 2.788(5) 136.2 2_665
O1W H1WB O3 0.85 2.13 2.788(5) 133.7 7
O3W H3WB N4 0.85 2.58 3.361(4) 153.8 13_655
O3W H3WB N3 0.85 2.62 3.339(3) 142.8 13_655
O3W H3WB N4 0.85 2.58 3.361(4) 153.8 13_655
