#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/63/7106359.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_7106359
loop_
_publ_author_name
'Ming-Hua Xie'
'Xiu-Li Yang'
'Chuan-De Wu'
_publ_section_title
;
 A metalloporphyrin functionalized metal–organic framework for
 selective oxidization of styrene
;
_journal_name_full               Chem.Commun.
_journal_page_first              5521
_journal_paper_doi               10.1039/c1cc10461f
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C64 H41 Cd1.25 N4 O8.5 Pd'
_chemical_formula_weight         1248.91
_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'
_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                 96.478(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2751(3)
_cell_length_b                   25.5905(15)
_cell_length_c                   30.7749(11)
_cell_measurement_reflns_used    9346
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      58.93
_cell_measurement_theta_min      3.45
_cell_volume                     5692.9(5)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'CrystalStructure and PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9346
_diffrn_reflns_theta_full        58.93
_diffrn_reflns_theta_max         58.93
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    6.754
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4037
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0969
_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)+(0.0796P)²+28.3160P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2234
_refine_ls_wR_factor_ref         0.2323
_reflns_number_gt                2852
_reflns_number_total             4037
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c1cc10461f.txt
_cod_data_source_block           New1c
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C64 H41 Cd1.25 N4 O8.50 Pd'
_cod_database_code               7106359
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_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
Cd1 Cd 0.5000 0.34427(5) 0.2500 0.1149(5) Uani 1 2 d S . .
Cd2 Cd 1.0000 0.2891(3) 0.2500 0.1442(19) Uani 0.25 2 d SPD . .
Pd1 Pd 1.5000 0.5000 0.0000 0.1079(5) Uani 1 2 d S . .
O1 O 0.7872(10) 0.3669(3) 0.2278(2) 0.119(2) Uani 1 1 d . . .
O2 O 0.5501(12) 0.4079(5) 0.1941(3) 0.154(3) Uani 1 1 d . . .
O3 O 0.889(3) 0.2409(9) -0.2027(8) 0.285(9) Uani 1 1 d DU . .
O5 O 1.0000 0.1993(5) 0.2500 0.42(4) Uani 0.25 2 d SPDU . .
N1 N 1.4468(12) 0.5284(4) 0.0588(3) 0.106(2) Uani 1 1 d . . .
N2 N 1.2905(13) 0.4504(4) -0.0001(3) 0.115(3) Uani 1 1 d . . .
C1 C 1.5381(17) 0.5675(5) 0.0816(4) 0.112(3) Uani 1 1 d . . .
C2 C 1.464(2) 0.5748(6) 0.1225(4) 0.130(4) Uani 1 1 d . . .
H2A H 1.5037 0.5988 0.1443 0.157 Uiso 1 1 calc R . .
C3 C 1.332(2) 0.5410(6) 0.1229(4) 0.128(4) Uani 1 1 d . . .
H3A H 1.2589 0.5373 0.1456 0.154 Uiso 1 1 calc R . .
C4 C 1.3117(16) 0.5094(6) 0.0833(3) 0.115(4) Uani 1 1 d . . .
C5 C 1.1862(15) 0.4705(6) 0.0714(3) 0.114(3) Uani 1 1 d . . .
C6 C 1.1728(17) 0.4445(5) 0.0332(4) 0.115(3) Uani 1 1 d . . .
C7 C 1.048(3) 0.4034(8) 0.0216(5) 0.175(6) Uani 1 1 d . . .
H7A H 0.9575 0.3912 0.0382 0.210 Uiso 1 1 calc R . .
C8 C 1.084(3) 0.3838(7) -0.0196(5) 0.172(6) Uani 1 1 d . . .
H8A H 1.0197 0.3575 -0.0357 0.207 Uiso 1 1 calc R . .
C9 C 1.2351(19) 0.4121(5) -0.0312(4) 0.123(4) Uani 1 1 d . . .
C10 C 1.3165(19) 0.4032(5) -0.0688(4) 0.122(3) Uani 1 1 d . . .
C11 C 1.0628(15) 0.4553(6) 0.1054(4) 0.120(4) Uani 1 1 d . . .
C12 C 1.1394(17) 0.4259(6) 0.1412(4) 0.137(5) Uani 1 1 d . . .
H12A H 1.2649 0.4178 0.1444 0.165 Uiso 1 1 calc R . .
C13 C 1.0276(16) 0.4090(6) 0.1716(4) 0.131(4) Uani 1 1 d . . .
H13A H 1.0788 0.3900 0.1958 0.157 Uiso 1 1 calc R . .
C14 C 0.8383(15) 0.4200(5) 0.1666(3) 0.105(3) Uani 1 1 d . . .
C15 C 0.7662(16) 0.4493(6) 0.1313(4) 0.128(4) Uani 1 1 d . . .
H15A H 0.6414 0.4581 0.1285 0.154 Uiso 1 1 calc R . .
C16 C 0.8739(15) 0.4660(6) 0.1003(4) 0.126(4) Uani 1 1 d . . .
H16A H 0.8211 0.4844 0.0760 0.151 Uiso 1 1 calc R . .
C17 C 0.7195(16) 0.3967(5) 0.1987(4) 0.111(3) Uani 1 1 d . . .
C18 C 1.242(2) 0.3594(4) -0.0992(3) 0.149(5) Uani 1 1 d G . .
C19 C 1.0676(19) 0.3635(5) -0.1227(4) 0.175(6) Uani 1 1 d G . .
H19A H 0.9955 0.3930 -0.1196 0.210 Uiso 1 1 calc R . .
C20 C 1.001(2) 0.3235(7) -0.1507(4) 0.228(11) Uani 1 1 d G . .
H20A H 0.8847 0.3262 -0.1664 0.274 Uiso 1 1 calc R . .
C21 C 1.109(3) 0.2794(5) -0.1553(4) 0.28(2) Uani 1 1 d GD . .
C22 C 1.283(3) 0.2753(5) -0.1318(5) 0.30(2) Uani 1 1 d G . .
H22A H 1.3555 0.2459 -0.1349 0.365 Uiso 1 1 calc R . .
C23 C 1.350(2) 0.3154(6) -0.1038(4) 0.226(11) Uani 1 1 d G . .
H23A H 1.4663 0.3126 -0.0881 0.271 Uiso 1 1 calc R . .
C24 C 1.049(3) 0.2366(7) -0.1891(5) 0.215(10) Uani 1 1 d D . .
O4 O 1.183(3) 0.2050(9) -0.1934(7) 0.310(9) Uani 1 1 d DU . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 '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
O1 Cd1 O1 151.4(4) . 2_655 ?
O1 Cd1 O4 110.8(6) . 7_655 ?
O1 Cd1 O4 84.4(6) 2_655 7_655 ?
O1 Cd1 O4 84.4(6) . 8_456 ?
O1 Cd1 O4 110.8(6) 2_655 8_456 ?
O4 Cd1 O4 117.3(11) 7_655 8_456 ?
O1 Cd1 O2 54.3(3) . . ?
O1 Cd1 O2 104.6(3) 2_655 . ?
O4 Cd1 O2 87.4(6) 7_655 . ?
O4 Cd1 O2 138.1(6) 8_456 . ?
O1 Cd1 O2 104.6(3) . 2_655 ?
O1 Cd1 O2 54.3(3) 2_655 2_655 ?
O4 Cd1 O2 138.1(6) 7_655 2_655 ?
O4 Cd1 O2 87.4(6) 8_456 2_655 ?
O2 Cd1 O2 95.7(5) . 2_655 ?
O1 Cd1 C17 26.9(3) . . ?
O1 Cd1 C17 130.4(4) 2_655 . ?
O4 Cd1 C17 98.7(6) 7_655 . ?
O4 Cd1 C17 111.2(6) 8_456 . ?
O2 Cd1 C17 27.5(3) . . ?
O2 Cd1 C17 103.1(4) 2_655 . ?
O1 Cd1 C17 130.4(4) . 2_655 ?
O1 Cd1 C17 26.9(3) 2_655 2_655 ?
O4 Cd1 C17 111.2(6) 7_655 2_655 ?
O4 Cd1 C17 98.7(6) 8_456 2_655 ?
O2 Cd1 C17 103.1(4) . 2_655 ?
O2 Cd1 C17 27.5(3) 2_655 2_655 ?
C17 Cd1 C17 120.9(5) . 2_655 ?
O5 Cd2 O1 140.8(2) . 2_755 ?
O5 Cd2 O1 140.8(2) . . ?
O1 Cd2 O1 78.3(4) 2_755 . ?
N2 Pd1 N2 180.0(5) 5_865 . ?
N2 Pd1 N1 90.4(4) 5_865 5_865 ?
N2 Pd1 N1 89.6(4) . 5_865 ?
N2 Pd1 N1 89.6(4) 5_865 . ?
N2 Pd1 N1 90.4(4) . . ?
N1 Pd1 N1 180.0(6) 5_865 . ?
C17 O1 Cd1 93.9(7) . . ?
C17 O1 Cd2 148.3(7) . . ?
Cd1 O1 Cd2 105.2(3) . . ?
C17 O2 Cd1 89.5(7) . . ?
C1 N1 C4 108.2(10) . . ?
C1 N1 Pd1 126.6(7) . . ?
C4 N1 Pd1 125.2(8) . . ?
C9 N2 C6 105.7(10) . . ?
C9 N2 Pd1 127.8(7) . . ?
C6 N2 Pd1 126.4(8) . . ?
N1 C1 C10 126.7(10) . 5_865 ?
N1 C1 C2 109.9(12) . . ?
C10 C1 C2 123.4(12) 5_865 . ?
C3 C2 C1 105.8(12) . . ?
C2 C3 C4 111.7(11) . . ?
C5 C4 N1 126.6(10) . . ?
C5 C4 C3 128.9(11) . . ?
N1 C4 C3 104.4(12) . . ?
C6 C5 C4 125.0(10) . . ?
C6 C5 C11 119.4(12) . . ?
C4 C5 C11 115.5(10) . . ?
C5 C6 C7 124.8(12) . . ?
C5 C6 N2 126.2(11) . . ?
C7 C6 N2 108.7(11) . . ?
C6 C7 C8 108.2(13) . . ?
C9 C8 C7 106.1(14) . . ?
C10 C9 C8 123.8(13) . . ?
C10 C9 N2 125.0(12) . . ?
C8 C9 N2 111.2(11) . . ?
C9 C10 C1 124.2(12) . 5_865 ?
C9 C10 C18 118.8(12) . . ?
C1 C10 C18 117.0(11) 5_865 . ?
C16 C11 C12 119.7(10) . . ?
C16 C11 C5 122.0(10) . . ?
C12 C11 C5 118.1(10) . . ?
C13 C12 C11 119.5(11) . . ?
C12 C13 C14 120.7(11) . . ?
C15 C14 C13 118.8(10) . . ?
C15 C14 C17 122.5(10) . . ?
C13 C14 C17 118.6(10) . . ?
C16 C15 C14 121.6(10) . . ?
C15 C16 C11 119.7(11) . . ?
O1 C17 O2 121.8(11) . . ?
O1 C17 C14 120.5(10) . . ?
O2 C17 C14 117.6(11) . . ?
O1 C17 Cd1 59.1(6) . . ?
O2 C17 Cd1 63.0(6) . . ?
C14 C17 Cd1 172.9(8) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C10 120.4(11) . . ?
C23 C18 C10 119.6(11) . . ?
C18 C19 C20 120.0 . . ?
C19 C20 C21 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 C24 118.2(16) . . ?
C20 C21 C24 121.6(16) . . ?
C21 C22 C23 120.0 . . ?
C22 C23 C18 120.0 . . ?
O3 C24 O4 138(2) . . ?
O3 C24 C21 111.4(19) . . ?
O4 C24 C21 110.6(19) . . ?
C24 O4 Cd1 92.2(13) . 7_655 ?
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
Cd1 O1 2.343(7) . ?
Cd1 O1 2.343(7) 2_655 ?
Cd1 O4 2.42(2) 7_655 ?
Cd1 O4 2.42(2) 8_456 ?
Cd1 O2 2.426(9) . ?
Cd1 O2 2.426(9) 2_655 ?
Cd1 C17 2.723(12) . ?
Cd1 C17 2.723(12) 2_655 ?
Cd2 O5 2.299(10) . ?
Cd2 O1 2.566(10) 2_755 ?
Cd2 O1 2.566(10) . ?
Pd1 N2 1.982(10) 5_865 ?
Pd1 N2 1.982(10) . ?
Pd1 N1 2.028(8) 5_865 ?
Pd1 N1 2.028(8) . ?
O1 C17 1.236(13) . ?
O2 C17 1.257(13) . ?
O3 C24 1.193(10) . ?
N1 C1 1.353(15) . ?
N1 C4 1.392(14) . ?
N2 C9 1.398(15) . ?
N2 C6 1.417(14) . ?
C1 C10 1.389(17) 5_865 ?
C1 C2 1.436(16) . ?
C2 C3 1.296(17) . ?
C3 C4 1.455(17) . ?
C4 C5 1.374(17) . ?
C5 C6 1.342(16) . ?
C5 C11 1.505(15) . ?
C6 C7 1.41(2) . ?
C7 C8 1.41(2) . ?
C8 C9 1.397(19) . ?
C9 C10 1.377(16) . ?
C10 C1 1.389(17) 5_865 ?
C10 C18 1.520(15) . ?
C11 C16 1.393(15) . ?
C11 C12 1.397(17) . ?
C12 C13 1.378(16) . ?
C13 C14 1.397(15) . ?
C14 C15 1.374(15) . ?
C14 C17 1.507(15) . ?
C15 C16 1.369(16) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C21 C24 1.540(10) . ?
C22 C23 1.3900 . ?
C24 O4 1.288(10) . ?
O4 Cd1 2.42(2) 7_655 ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.109 0.250 0.000 357 67 ' '
2 0.047 0.750 0.000 357 67 ' '
3 -0.013 0.573 0.250 230 47 ' '
4 -0.022 0.073 0.250 230 47 ' '
5 -0.088 0.750 0.500 357 67 ' '
6 0.104 0.250 0.500 357 67 ' '
7 -0.013 0.427 0.750 230 47 ' '
8 -0.022 0.927 0.750 230 47 ' '
