#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/63/7106356.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_7106356
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            'C54 H41.5 Cd1.25 N6 O11 Pd'
_chemical_formula_weight         1197.33
_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                 96.361(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.29530(10)
_cell_length_b                   25.5761(7)
_cell_length_c                   30.7597(6)
_cell_measurement_reflns_used    15512
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      58.91
_cell_measurement_theta_min      3.46
_cell_volume                     5704.0(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15512
_diffrn_reflns_theta_full        58.91
_diffrn_reflns_theta_max         58.91
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    6.756
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2406
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4054
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0776
_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)+(0.0867P)²+21.1888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.1904
_reflns_number_gt                3395
_reflns_number_total             4054
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c1cc10461f.txt
_cod_data_source_block           New1
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C54 H41.50 Cd1.25 N6 O11 Pd'
_cod_database_code               7106356
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 0.34476(3) 0.2500 0.0995(3) Uani 1 2 d S . .
Cd2 Cd 1.0000 0.2909(2) 0.2500 0.1441(16) Uani 0.25 2 d SPD . .
Pd1 Pd 1.5000 0.5000 0.0000 0.0954(3) Uani 1 2 d S . .
O1 O 0.7851(8) 0.3686(3) 0.22808(18) 0.1140(17) Uani 1 1 d . . .
O2 O 0.5485(9) 0.4081(3) 0.1943(2) 0.142(3) Uani 1 1 d . . .
O3 O 0.913(4) 0.2360(7) -0.2022(6) 0.357(18) Uani 1 1 d D . .
O4 O 1.197(4) 0.2027(5) -0.1961(4) 0.366(17) Uani 1 1 d D . .
O5 O 0.991(5) 0.2418(15) 0.3074(9) 0.303(15) Uani 0.25 1 d PD . .
N1 N 1.4447(9) 0.5295(3) 0.05850(19) 0.0964(17) Uani 1 1 d . . .
N2 N 1.2867(9) 0.4502(3) -0.0003(2) 0.0998(17) Uani 1 1 d . . .
C1 C 1.5364(13) 0.5692(4) 0.0816(3) 0.101(2) Uani 1 1 d . . .
C2 C 1.4591(16) 0.5756(5) 0.1223(3) 0.127(3) Uani 1 1 d . . .
H2A H 1.4974 0.5994 0.1443 0.153 Uiso 1 1 calc R . .
C3 C 1.3246(14) 0.5417(5) 0.1224(3) 0.123(3) Uani 1 1 d . . .
H3A H 1.2499 0.5379 0.1448 0.147 Uiso 1 1 calc R . .
C4 C 1.3093(12) 0.5114(4) 0.0832(3) 0.107(2) Uani 1 1 d . . .
C5 C 1.1839(11) 0.4725(4) 0.0713(3) 0.103(2) Uani 1 1 d . . .
C6 C 1.1709(12) 0.4447(4) 0.0320(3) 0.106(2) Uani 1 1 d . . .
C7 C 1.0463(18) 0.4047(5) 0.0203(4) 0.149(4) Uani 1 1 d . . .
H7A H 0.9528 0.3936 0.0364 0.179 Uiso 1 1 calc R . .
C8 C 1.0835(18) 0.3845(5) -0.0182(4) 0.146(4) Uani 1 1 d . . .
H8A H 1.0233 0.3568 -0.0333 0.175 Uiso 1 1 calc R . .
C9 C 1.2316(14) 0.4137(4) -0.0309(3) 0.113(3) Uani 1 1 d . . .
C10 C 1.3174(14) 0.4033(4) -0.0695(3) 0.110(2) Uani 1 1 d . . .
C11 C 1.0624(11) 0.4553(4) 0.1050(3) 0.107(2) Uani 1 1 d . . .
C12 C 1.1363(12) 0.4282(4) 0.1417(3) 0.121(3) Uani 1 1 d . . .
H12A H 1.2621 0.4213 0.1458 0.145 Uiso 1 1 calc R . .
C13 C 1.0252(12) 0.4116(4) 0.1719(3) 0.118(3) Uani 1 1 d . . .
H13A H 1.0773 0.3939 0.1966 0.142 Uiso 1 1 calc R . .
C14 C 0.8373(11) 0.4204(4) 0.1664(2) 0.102(2) Uani 1 1 d . . .
C15 C 0.7642(12) 0.4481(4) 0.1305(3) 0.111(3) Uani 1 1 d . . .
H15A H 0.6387 0.4556 0.1267 0.133 Uiso 1 1 calc R . .
C16 C 0.8749(12) 0.4646(4) 0.1002(3) 0.116(3) Uani 1 1 d . . .
H16A H 0.8225 0.4826 0.0756 0.139 Uiso 1 1 calc R . .
C17 C 0.7153(12) 0.3975(4) 0.1987(3) 0.104(2) Uani 1 1 d . . .
C18 C 1.2470(14) 0.3592(3) -0.0981(2) 0.137(4) Uani 1 1 d G . .
C19 C 1.0731(13) 0.3619(3) -0.1216(3) 0.160(4) Uani 1 1 d G . .
H19A H 0.9972 0.3905 -0.1181 0.191 Uiso 1 1 calc R . .
C20 C 1.0126(14) 0.3218(5) -0.1502(3) 0.188(6) Uani 1 1 d G . .
H20A H 0.8962 0.3236 -0.1659 0.225 Uiso 1 1 calc R . .
C21 C 1.126(2) 0.2791(4) -0.1554(3) 0.236(11) Uani 1 1 d GD . .
C22 C 1.300(2) 0.2765(3) -0.1319(4) 0.273(14) Uani 1 1 d G . .
H22A H 1.3758 0.2479 -0.1354 0.328 Uiso 1 1 calc R . .
C23 C 1.3604(15) 0.3165(4) -0.1033(3) 0.204(8) Uani 1 1 d G . .
H23A H 1.4767 0.3147 -0.0876 0.245 Uiso 1 1 calc R . .
C24 C 1.072(4) 0.2363(8) -0.1888(6) 0.244(13) Uani 1 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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 149.8(4) . 2_655 ?
O1 Cd1 O4 81.2(7) . 8_456 ?
O1 Cd1 O4 114.6(6) 2_655 8_456 ?
O1 Cd1 O4 114.6(6) . 7_655 ?
O1 Cd1 O4 81.2(7) 2_655 7_655 ?
O4 Cd1 O4 119.3(7) 8_456 7_655 ?
O1 Cd1 O2 103.6(2) . 2_655 ?
O1 Cd1 O2 54.2(2) 2_655 2_655 ?
O4 Cd1 O2 88.4(4) 8_456 2_655 ?
O4 Cd1 O2 134.9(6) 7_655 2_655 ?
O1 Cd1 O2 54.2(2) . . ?
O1 Cd1 O2 103.6(2) 2_655 . ?
O4 Cd1 O2 134.9(6) 8_456 . ?
O4 Cd1 O2 88.4(4) 7_655 . ?
O2 Cd1 O2 95.6(4) 2_655 . ?
O1 Cd1 O3 129.6(5) . 8_456 ?
O1 Cd1 O3 76.6(5) 2_655 8_456 ?
O4 Cd1 O3 52.1(4) 8_456 8_456 ?
O4 Cd1 O3 80.1(6) 7_655 8_456 ?
O2 Cd1 O3 93.8(5) 2_655 8_456 ?
O2 Cd1 O3 168.4(5) . 8_456 ?
O1 Cd1 O3 76.6(5) . 7_655 ?
O1 Cd1 O3 129.6(5) 2_655 7_655 ?
O4 Cd1 O3 80.1(6) 8_456 7_655 ?
O4 Cd1 O3 52.1(4) 7_655 7_655 ?
O2 Cd1 O3 168.4(5) 2_655 7_655 ?
O2 Cd1 O3 93.8(5) . 7_655 ?
O3 Cd1 O3 77.7(9) 8_456 7_655 ?
O1 Cd1 C17 27.1(2) . . ?
O1 Cd1 C17 129.1(3) 2_655 . ?
O4 Cd1 C17 108.2(7) 8_456 . ?
O4 Cd1 C17 101.0(5) 7_655 . ?
O2 Cd1 C17 102.7(3) 2_655 . ?
O2 Cd1 C17 27.2(2) . . ?
O3 Cd1 C17 154.3(5) 8_456 . ?
O3 Cd1 C17 82.8(5) 7_655 . ?
O1 Cd1 C17 129.1(3) . 2_655 ?
O1 Cd1 C17 27.1(2) 2_655 2_655 ?
O4 Cd1 C17 101.0(5) 8_456 2_655 ?
O4 Cd1 C17 108.2(7) 7_655 2_655 ?
O2 Cd1 C17 27.2(2) 2_655 2_655 ?
O2 Cd1 C17 102.7(3) . 2_655 ?
O3 Cd1 C17 82.8(5) 8_456 2_655 ?
O3 Cd1 C17 154.3(5) 7_655 2_655 ?
C17 Cd1 C17 120.2(4) . 2_655 ?
O5 Cd2 O5 109(2) . 2_755 ?
O5 Cd2 O1 125.9(12) . . ?
O5 Cd2 O1 107.7(10) 2_755 . ?
O5 Cd2 O1 107.7(10) . 2_755 ?
O5 Cd2 O1 125.9(12) 2_755 2_755 ?
O1 Cd2 O1 79.0(3) . 2_755 ?
N2 Pd1 N2 179.999(1) 5_865 . ?
N2 Pd1 N1 89.4(3) 5_865 . ?
N2 Pd1 N1 90.6(3) . . ?
N2 Pd1 N1 90.6(3) 5_865 5_865 ?
N2 Pd1 N1 89.4(3) . 5_865 ?
N1 Pd1 N1 180.00(14) . 5_865 ?
C17 O1 Cd1 93.4(5) . . ?
C17 O1 Cd2 147.7(6) . . ?
Cd1 O1 Cd2 105.0(2) . . ?
C17 O2 Cd1 89.7(5) . . ?
C24 O3 Cd1 85.0(12) . 7_655 ?
C24 O4 Cd1 94.3(10) . 7_655 ?
C1 N1 C4 107.5(7) . . ?
C1 N1 Pd1 126.9(5) . . ?
C4 N1 Pd1 125.6(6) . . ?
C9 N2 C6 105.9(7) . . ?
C9 N2 Pd1 127.5(5) . . ?
C6 N2 Pd1 126.5(6) . . ?
C10 C1 N1 126.4(7) 5_865 . ?
C10 C1 C2 124.9(9) 5_865 . ?
N1 C1 C2 108.7(9) . . ?
C3 C2 C1 107.0(9) . . ?
C2 C3 C4 110.2(8) . . ?
C5 C4 N1 126.0(8) . . ?
C5 C4 C3 127.3(8) . . ?
N1 C4 C3 106.6(9) . . ?
C4 C5 C6 125.4(7) . . ?
C4 C5 C11 116.9(8) . . ?
C6 C5 C11 117.4(8) . . ?
N2 C6 C7 108.8(8) . . ?
N2 C6 C5 125.7(8) . . ?
C7 C6 C5 125.4(8) . . ?
C8 C7 C6 108.7(9) . . ?
C7 C8 C9 106.2(10) . . ?
N2 C9 C8 110.5(8) . . ?
N2 C9 C10 125.7(8) . . ?
C8 C9 C10 123.7(9) . . ?
C1 C10 C9 124.0(8) 5_865 . ?
C1 C10 C18 117.3(8) 5_865 . ?
C9 C10 C18 118.7(9) . . ?
C12 C11 C16 117.8(7) . . ?
C12 C11 C5 120.2(7) . . ?
C16 C11 C5 121.9(7) . . ?
C13 C12 C11 120.3(8) . . ?
C12 C13 C14 121.5(8) . . ?
C15 C14 C13 118.3(7) . . ?
C15 C14 C17 121.4(7) . . ?
C13 C14 C17 120.2(8) . . ?
C16 C15 C14 120.3(8) . . ?
C15 C16 C11 121.8(8) . . ?
O1 C17 O2 122.1(8) . . ?
O1 C17 C14 119.0(8) . . ?
O2 C17 C14 118.9(8) . . ?
O1 C17 Cd1 59.5(4) . . ?
O2 C17 Cd1 63.1(5) . . ?
C14 C17 Cd1 172.4(6) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C10 120.4(8) . . ?
C23 C18 C10 119.5(8) . . ?
C18 C19 C20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 C24 122.0(13) . . ?
C22 C21 C24 117.8(13) . . ?
C23 C22 C21 120.0 . . ?
C22 C23 C18 120.0 . . ?
O3 C24 O4 128.1(16) . . ?
O3 C24 C21 114.1(16) . . ?
O4 C24 C21 117.5(15) . . ?
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 2.337(5) . ?
Cd1 O1 2.337(5) 2_655 ?
Cd1 O4 2.402(16) 8_456 ?
Cd1 O4 2.402(16) 7_655 ?
Cd1 O2 2.414(7) 2_655 ?
Cd1 O2 2.414(7) . ?
Cd1 O3 2.65(2) 8_456 ?
Cd1 O3 2.652(19) 7_655 ?
Cd1 C17 2.708(9) . ?
Cd1 C17 2.708(9) 2_655 ?
Cd2 O5 2.174(10) . ?
Cd2 O5 2.174(10) 2_755 ?
Cd2 O1 2.574(8) . ?
Cd2 O1 2.574(8) 2_755 ?
Pd1 N2 2.011(7) 5_865 ?
Pd1 N2 2.011(7) . ?
Pd1 N1 2.032(6) . ?
Pd1 N1 2.033(6) 5_865 ?
O1 C17 1.235(10) . ?
O2 C17 1.239(10) . ?
O3 C24 1.188(10) . ?
O3 Cd1 2.652(19) 7_655 ?
O4 C24 1.292(10) . ?
O4 Cd1 2.402(16) 7_655 ?
N1 C1 1.370(11) . ?
N1 C4 1.390(10) . ?
N2 C9 1.354(11) . ?
N2 C6 1.381(10) . ?
C1 C10 1.364(13) 5_865 ?
C1 C2 1.439(12) . ?
C2 C3 1.310(14) . ?
C3 C4 1.429(13) . ?
C4 C5 1.374(13) . ?
C5 C6 1.394(12) . ?
C5 C11 1.503(11) . ?
C6 C7 1.389(14) . ?
C7 C8 1.346(15) . ?
C8 C9 1.404(14) . ?
C9 C10 1.426(12) . ?
C10 C1 1.364(13) 5_865 ?
C10 C18 1.487(11) . ?
C11 C12 1.381(12) . ?
C11 C16 1.380(11) . ?
C12 C13 1.367(12) . ?
C13 C14 1.381(11) . ?
C14 C15 1.371(11) . ?
C14 C17 1.521(12) . ?
C15 C16 1.366(12) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C21 C24 1.523(10) . ?
C22 C23 1.3900 . ?
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 -0.111 0.250 0.000 364 56 ' '
2 0.048 0.750 0.000 364 56 ' '
3 -0.017 0.579 0.250 242 36 ' '
4 -0.017 0.079 0.250 242 36 ' '
5 -0.085 0.750 0.500 363 56 ' '
6 0.090 0.250 0.501 363 56 ' '
7 -0.016 0.422 0.750 242 36 ' '
8 -0.018 0.922 0.750 242 36 ' '
