#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:39:32 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232247 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/72/4347291.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_4347291
loop_
_publ_author_name
'Chen, Gong-Jun'
'Wang, Jing-Si'
'Jin, Fa-Zheng'
'Liu, Ming-Yang'
'Zhao, Chao-Wei'
'Li, Yan-An'
'Dong, Yu-Bin'
_publ_section_title
;
 Pd@Cu(II)-MOF-Catalyzed Aerobic Oxidation of Benzylic Alcohols in Air
 with High Conversion and Selectivity.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3058
_journal_page_last               3064
_journal_paper_doi               10.1021/acs.inorgchem.5b02973
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C96 H54 Cu3 F18 N6 O18'
_chemical_formula_weight         2112.10
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            1
_cell_length_a                   21.5669(5)
_cell_length_b                   21.5669(5)
_cell_length_c                   7.7969(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3140.71(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7201
_diffrn_reflns_theta_full        71.06
_diffrn_reflns_theta_max         71.06
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    1.291
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1065
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0871
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2745
_refine_ls_wR_factor_ref         0.2433
_reflns_number_gt                3053
_reflns_number_total             4066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02973_si_002.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               4347291
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
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
Cu1 Cu 0.5000 0.0000 0.0000 0.0435(3) Uani 1 2 d S
F1 F 0.4067(2) 0.05394(19) -0.4716(4) 0.1006(12) Uani 1 1 d .
F2 F 0.3076(2) -0.0046(2) -0.3302(6) 0.1093(12) Uani 1 1 d .
F3 F 0.3625(2) 0.11042(18) -0.3423(4) 0.0928(11) Uani 1 1 d .
O1 O 0.42226(18) 0.00073(15) -0.1622(4) 0.0606(8) Uani 1 1 d .
O2 O 0.50349(19) 0.08603(17) 0.1406(4) 0.0652(9) Uani 1 1 d .
N1 N 0.49523(19) 0.42559(19) 0.8356(4) 0.0511(8) Uani 1 1 d .
C1 C 0.4860(2) 0.4326(2) 0.6676(4) 0.0473(9) Uani 1 1 d .
H1 H 0.4804 0.4708 0.6324 0.057 Uiso 1 1 calc R
C2 C 0.4843(2) 0.3861(2) 0.5466(4) 0.0486(9) Uani 1 1 d .
H2 H 0.4773 0.3926 0.4319 0.058 Uiso 1 1 calc R
C3 C 0.4931(3) 0.3288(2) 0.5952(5) 0.0552(10) Uani 1 1 d .
C4 C 0.5047(3) 0.3712(3) 0.8822(5) 0.0757(15) Uani 1 1 d .
H4 H 0.5119 0.3661 0.9977 0.091 Uiso 1 1 calc R
C5 C 0.5043(4) 0.3227(3) 0.7680(6) 0.0794(16) Uani 1 1 d .
H5 H 0.5116 0.2860 0.8061 0.095 Uiso 1 1 calc R
C6 C 0.4904(3) 0.2775(2) 0.4645(5) 0.0603(11) Uani 1 1 d .
C7 C 0.4447(3) 0.2596(3) 0.3244(5) 0.0635(12) Uani 1 1 d .
H7 H 0.4178 0.2821 0.3107 0.076 Uiso 1 1 calc R
C8 C 0.4383(3) 0.2097(3) 0.2056(5) 0.0649(12) Uani 1 1 d .
H8 H 0.4059 0.1975 0.1156 0.078 Uiso 1 1 calc R
C9 C 0.4805(3) 0.1770(3) 0.2198(5) 0.0644(12) Uani 1 1 d .
C10 C 0.5292(3) 0.1977(3) 0.3563(6) 0.0760(15) Uani 1 1 d .
H10 H 0.5586 0.1778 0.3655 0.091 Uiso 1 1 calc R
C11 C 0.5343(3) 0.2466(3) 0.4769(6) 0.0752(15) Uani 1 1 d .
H11 H 0.5668 0.2592 0.5667 0.090 Uiso 1 1 calc R
C12 C 0.4741(3) 0.1218(2) 0.0969(6) 0.0658(12) Uani 1 1 d .
C13 C 0.4365(3) 0.1120(3) -0.0609(6) 0.0695(13) Uani 1 1 d .
H13 H 0.4262 0.1475 -0.0924 0.083 Uiso 1 1 calc R
C14 C 0.4145(3) 0.0550(3) -0.1694(6) 0.0661(12) Uani 1 1 d .
C15 C 0.3738(4) 0.0550(3) -0.3289(7) 0.0810(15) Uani 1 1 d .
O3 O 0.6331(6) 0.3108(10) 1.066(2) 0.316(9) Uani 1 1 d .
C16 C 0.6252(8) 0.2763(7) 0.8598(16) 0.191(6) Uani 1 1 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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
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
N1 Cu1 N1 180.0(4) 5_556 2_654
N1 Cu1 O1 92.71(13) 5_556 .
N1 Cu1 O1 87.29(13) 2_654 .
N1 Cu1 O1 87.29(13) 5_556 4_655
N1 Cu1 O1 92.71(13) 2_654 4_655
O1 Cu1 O1 180.00(19) . 4_655
N1 Cu1 O2 89.42(12) 5_556 .
N1 Cu1 O2 90.58(12) 2_654 .
O1 Cu1 O2 89.09(11) . .
O1 Cu1 O2 90.91(11) 4_655 .
N1 Cu1 O2 90.58(12) 5_556 4_655
N1 Cu1 O2 89.42(12) 2_654 4_655
O1 Cu1 O2 90.91(11) . 4_655
O1 Cu1 O2 89.09(11) 4_655 4_655
O2 Cu1 O2 180.0(2) . 4_655
C14 O1 Cu1 120.5(3) . .
C12 O2 Cu1 125.7(3) . .
C4 N1 C1 117.4(4) . .
C4 N1 Cu1 123.8(3) . 3_666
C1 N1 Cu1 118.7(3) . 3_666
N1 C1 C2 122.8(3) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C1 C2 C3 119.9(3) . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C5 C3 C2 117.1(4) . .
C5 C3 C6 122.7(4) . .
C2 C3 C6 120.2(3) . .
N1 C4 C5 123.2(4) . .
N1 C4 H4 118.4 . .
C5 C4 H4 118.4 . .
C4 C5 C3 119.6(4) . .
C4 C5 H5 120.2 . .
C3 C5 H5 120.2 . .
C7 C6 C11 118.2(4) . .
C7 C6 C3 120.3(4) . .
C11 C6 C3 121.4(4) . .
C8 C7 C6 121.9(4) . .
C8 C7 H7 119.1 . .
C6 C7 H7 119.1 . .
C7 C8 C9 120.1(4) . .
C7 C8 H8 119.9 . .
C9 C8 H8 119.9 . .
C10 C9 C8 118.0(4) . .
C10 C9 C12 120.0(4) . .
C8 C9 C12 121.9(4) . .
C11 C10 C9 121.6(4) . .
C11 C10 H10 119.2 . .
C9 C10 H10 119.2 . .
C10 C11 C6 120.0(5) . .
C10 C11 H11 120.0 . .
C6 C11 H11 120.0 . .
O2 C12 C13 124.2(4) . .
O2 C12 C9 116.3(4) . .
C13 C12 C9 119.5(4) . .
C14 C13 C12 125.5(4) . .
C14 C13 H13 117.2 . .
C12 C13 H13 117.2 . .
O1 C14 C13 131.2(5) . .
O1 C14 C15 112.3(4) . .
C13 C14 C15 116.5(4) . .
F1 C15 F3 106.7(4) . .
F1 C15 F2 107.1(5) . .
F3 C15 F2 105.7(5) . .
F1 C15 C14 111.7(5) . .
F3 C15 C14 115.3(4) . .
F2 C15 C14 109.8(4) . .
O3 O3 O3 60.000(16) 3_665 2_655
O3 O3 C16 108.2(6) 3_665 .
O3 O3 C16 87.7(15) 2_655 .
O3 C16 C16 67.3(9) . 3_665
O3 C16 C16 79.6(5) . 2_655
C16 C16 C16 60.000(5) 3_665 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.016(3) 5_556
Cu1 N1 2.016(3) 2_654
Cu1 O1 2.107(3) .
Cu1 O1 2.107(3) 4_655
Cu1 O2 2.124(3) .
Cu1 O2 2.124(3) 4_655
F1 C15 1.327(6) .
F2 C15 1.362(7) .
F3 C15 1.337(6) .
O1 C14 1.263(5) .
O2 C12 1.265(5) .
N1 C4 1.337(5) .
N1 C1 1.345(4) .
N1 Cu1 2.016(3) 3_666
C1 C2 1.364(5) .
C1 H1 0.9300 .
C2 C3 1.394(5) .
C2 H2 0.9300 .
C3 C5 1.386(6) .
C3 C6 1.483(6) .
C4 C5 1.371(7) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C7 1.391(6) .
C6 C11 1.408(6) .
C7 C8 1.373(6) .
C7 H7 0.9300 .
C8 C9 1.407(6) .
C8 H8 0.9300 .
C9 C10 1.402(7) .
C9 C12 1.482(6) .
C10 C11 1.376(7) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C12 C13 1.430(7) .
C13 C14 1.367(6) .
C13 H13 0.9300 .
C14 C15 1.523(7) .
O3 O3 1.107(16) 3_665
O3 O3 1.107(16) 2_655
O3 C16 1.745(17) .
C16 C16 1.91(2) 3_665
C16 C16 1.91(2) 2_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Cu1 O1 C14 108.3(3) 5_556 .
N1 Cu1 O1 C14 -71.7(3) 2_654 .
O1 Cu1 O1 C14 -105(45) 4_655 .
O2 Cu1 O1 C14 18.9(3) . .
O2 Cu1 O1 C14 -161.1(3) 4_655 .
N1 Cu1 O2 C12 -102.6(4) 5_556 .
N1 Cu1 O2 C12 77.4(4) 2_654 .
O1 Cu1 O2 C12 -9.9(4) . .
O1 Cu1 O2 C12 170.1(4) 4_655 .
O2 Cu1 O2 C12 54.5(4) 4_655 .
C4 N1 C1 C2 1.5(7) . .
Cu1 N1 C1 C2 177.9(3) 3_666 .
N1 C1 C2 C3 -0.6(6) . .
C1 C2 C3 C5 -0.9(7) . .
C1 C2 C3 C6 179.2(4) . .
C1 N1 C4 C5 -0.9(8) . .
Cu1 N1 C4 C5 -177.1(5) 3_666 .
N1 C4 C5 C3 -0.6(10) . .
C2 C3 C5 C4 1.5(9) . .
C6 C3 C5 C4 -178.7(5) . .
C5 C3 C6 C7 145.3(5) . .
C2 C3 C6 C7 -34.8(7) . .
C5 C3 C6 C11 -35.6(8) . .
C2 C3 C6 C11 144.3(5) . .
C11 C6 C7 C8 4.2(8) . .
C3 C6 C7 C8 -176.7(4) . .
C6 C7 C8 C9 -2.5(8) . .
C7 C8 C9 C10 -0.7(8) . .
C7 C8 C9 C12 178.6(4) . .
C8 C9 C10 C11 2.1(8) . .
C12 C9 C10 C11 -177.2(5) . .
C9 C10 C11 C6 -0.4(9) . .
C7 C6 C11 C10 -2.8(8) . .
C3 C6 C11 C10 178.1(5) . .
Cu1 O2 C12 C13 -3.4(7) . .
Cu1 O2 C12 C9 176.9(3) . .
C10 C9 C12 O2 13.1(7) . .
C8 C9 C12 O2 -166.2(5) . .
C10 C9 C12 C13 -166.6(5) . .
C8 C9 C12 C13 14.1(7) . .
O2 C12 C13 C14 13.9(9) . .
C9 C12 C13 C14 -166.4(5) . .
Cu1 O1 C14 C13 -17.3(7) . .
Cu1 O1 C14 C15 162.3(4) . .
C12 C13 C14 O1 -1.7(10) . .
C12 C13 C14 C15 178.7(5) . .
O1 C14 C15 F1 -59.2(6) . .
C13 C14 C15 F1 120.5(5) . .
O1 C14 C15 F3 178.7(5) . .
C13 C14 C15 F3 -1.6(8) . .
O1 C14 C15 F2 59.5(6) . .
C13 C14 C15 F2 -120.8(5) . .
O3 O3 C16 C16 -36(3) 3_665 3_665
O3 O3 C16 C16 -93(2) 2_655 3_665
O3 O3 C16 C16 26(3) 3_665 2_655
O3 O3 C16 C16 -32(2) 2_655 2_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 0.000 1.000 0.500 315 45 ' '
