#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:29:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179020 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/18/4121854.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_4121854
loop_
_publ_author_name
'Li, Liangchun'
'Matsuda, Ryotaro'
'Tanaka, Iku'
'Sato, Hiroshi'
'Kanoo, Prakash'
'Jeon, Hyung Joon'
'Foo, Maw Lin'
'Wakamiya, Atsushi'
'Murata, Yasujiro'
'Kitagawa, Susumu'
_publ_section_title
;
 A crystalline porous coordination polymer decorated with nitroxyl
 radicals catalyzes aerobic oxidation of alcohols.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7543
_journal_page_last               7546
_journal_paper_doi               10.1021/ja5019095
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         C44H44CuF6N6O6Si
_chemical_formula_sum            'C44 H44 Cu F6 N6 O6 Si'
_chemical_formula_weight         958.48
_chemical_name_common            FRPCP
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           108
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      108
_symmetry_space_group_name_Hall  'I 4 -2c'
_symmetry_space_group_name_H-M   'I 4 c 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                   21.682(11)
_cell_length_b                   21.682(11)
_cell_length_c                   15.696(8)
_cell_measurement_reflns_used    7713
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.4498
_cell_measurement_theta_min      1.6017
_cell_volume                     7379(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1494
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34941
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.9822
_exptl_absorpt_correction_T_min  0.9683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    0.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.83(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3386
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.1145
_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)+(0.0500P)²+100.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2378
_reflns_number_gt                2819
_reflns_number_total             3386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5019095_si_003.cif
_cod_data_source_block           FRPCP
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4121853--4121854.cif.
;
_cod_database_code               4121854
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, z+1/2'
'x, -y, z+1/2'
'y, x, z+1/2'
'-y, -x, z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'y+1/2, x+1/2, z+1'
'-y+1/2, -x+1/2, z+1'
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
F1 F 0.0000 0.0000 0.5186(5) 0.024(2) Uani 1 4 d S
F2 F -0.02147(19) 0.07449(16) 0.4087(5) 0.0394(11) Uani 1 1 d .
F3 F 0.0000 0.0000 0.3023(6) 0.0280(15) Uani 1 4 d SU
C1 C -0.0938(4) 0.0877(4) 0.5993(5) 0.0368(15) Uani 1 1 d U
H1 H -0.0940 0.0627 0.5496 0.044 Uiso 1 1 calc R
C2 C -0.1358(5) 0.1355(5) 0.6051(6) 0.0479(16) Uani 1 1 d U
H2 H -0.1650 0.1410 0.5606 0.057 Uiso 1 1 calc R
C3 C -0.1367(4) 0.1731(4) 0.6696(7) 0.0513(15) Uani 1 1 d U
C4 C -0.0913(4) 0.1664(4) 0.7326(6) 0.0489(16) Uani 1 1 d U
H4 H -0.0885 0.1948 0.7785 0.059 Uiso 1 1 calc R
C5 C -0.0494(4) 0.1159(4) 0.7261(5) 0.0347(16) Uani 1 1 d U
H5 H -0.0183 0.1100 0.7680 0.042 Uiso 1 1 calc R
C6 C -0.1850(5) 0.2240(5) 0.6773(6) 0.0566(17) Uani 1 1 d U
C7 C -0.1822(5) 0.2705(5) 0.6275(7) 0.060(2) Uani 1 1 d U
H7 H -0.1482 0.2742 0.5895 0.072 Uiso 1 1 calc R
C8 C -0.2341(5) 0.2199(5) 0.7393(7) 0.0618(18) Uani 1 1 d U
C9 C -0.2472(6) 0.1707(5) 0.8055(7) 0.0724(19) Uani 1 1 d U
C10 C -0.2548(6) 0.1054(5) 0.7721(8) 0.072(2) Uani 1 1 d U
H10 H -0.2783 0.1062 0.7187 0.108 Uiso 1 1 calc R
H10A H -0.2770 0.0805 0.8142 0.108 Uiso 1 1 calc R
H10B H -0.2141 0.0873 0.7617 0.108 Uiso 1 1 calc R
C11 C -0.2047(5) 0.1695(6) 0.8860(7) 0.074(2) Uani 1 1 d U
H11 H -0.1677 0.1452 0.8738 0.111 Uiso 1 1 calc R
H11A H -0.2271 0.1509 0.9338 0.111 Uiso 1 1 calc R
H11B H -0.1928 0.2118 0.9009 0.111 Uiso 1 1 calc R
Cu1 Cu 0.0000 0.0000 0.66057(14) 0.0202(4) Uani 1 4 d S
Si1 Si 0.0000 0.0000 0.4107(4) 0.0214(6) Uani 1 4 d S
N1 N -0.0545(2) 0.0757(2) 0.6586(5) 0.0208(10) Uani 1 1 d U
N2 N -0.3066(5) 0.1934(5) 0.8412(10) 0.0762(16) Uani 1 2 d SU
O1 O -0.3359(6) 0.1641(6) 0.9000(11) 0.146(7) Uani 1 2 d S
O2 O 0.0251(7) 0.1947(6) 0.4399(10) 0.201(8) 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 0.0033 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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
Si1 F1 Cu1 180.000(1) . .
Si1 F3 Cu1 180.000(1) . 5_554
N1 C1 C2 122.6(8) . .
N1 C1 H1 118.7 . .
C2 C1 H1 118.7 . .
C3 C2 C1 122.1(9) . .
C3 C2 H2 118.9 . .
C1 C2 H2 118.9 . .
C2 C3 C4 118.2(8) . .
C2 C3 C6 121.7(9) . .
C4 C3 C6 120.0(9) . .
C3 C4 C5 118.4(9) . .
C3 C4 H4 120.8 . .
C5 C4 H4 120.8 . .
N1 C5 C4 119.4(8) . .
N1 C5 H5 120.3 . .
C4 C5 H5 120.3 . .
C7 C6 C8 119.8(9) . .
C7 C6 C3 119.3(9) . .
C8 C6 C3 120.9(9) . .
C6 C7 C7 121.6(6) . 15_454
C6 C7 H7 119.2 . .
C7 C7 H7 119.2 15_454 .
C8 C8 C6 118.5(5) 15_454 .
C8 C8 C9 111.4(6) 15_454 .
C6 C8 C9 130.1(9) . .
N2 C9 C8 100.9(9) . .
N2 C9 C10 110.2(11) . .
C8 C9 C10 116.1(9) . .
N2 C9 C11 102.2(10) . .
C8 C9 C11 117.0(11) . .
C10 C9 C11 109.1(9) . .
C9 C10 H10 109.5 . .
C9 C10 H10A 109.5 . .
H10 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C11 H11 109.5 . .
C9 C11 H11A 109.5 . .
H11 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
H11 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N1 Cu1 N1 178.2(5) 4 3
N1 Cu1 N1 89.986(8) 4 2
N1 Cu1 N1 89.986(9) 3 2
N1 Cu1 N1 89.987(9) 4 .
N1 Cu1 N1 89.986(8) 3 .
N1 Cu1 N1 178.2(5) 2 .
N1 Cu1 F3 90.9(2) 4 5
N1 Cu1 F3 90.9(2) 3 5
N1 Cu1 F3 90.9(2) 2 5
N1 Cu1 F3 90.9(2) . 5
N1 Cu1 F1 89.1(2) 4 .
N1 Cu1 F1 89.1(2) 3 .
N1 Cu1 F1 89.1(2) 2 .
N1 Cu1 F1 89.1(2) . .
F3 Cu1 F1 180.000(2) 5 .
F2 Si1 F2 89.983(14) . 4
F2 Si1 F2 89.978(14) . 3
F2 Si1 F2 177.9(7) 4 3
F2 Si1 F2 177.9(7) . 2
F2 Si1 F2 89.981(13) 4 2
F2 Si1 F2 89.981(14) 3 2
F2 Si1 F1 91.1(3) . .
F2 Si1 F1 91.1(3) 4 .
F2 Si1 F1 91.1(3) 3 .
F2 Si1 F1 91.1(3) 2 .
F2 Si1 F3 88.9(3) . .
F2 Si1 F3 88.9(3) 4 .
F2 Si1 F3 88.9(3) 3 .
F2 Si1 F3 88.9(3) 2 .
F1 Si1 F3 180.000(2) . .
C1 N1 C5 118.7(6) . .
C1 N1 Cu1 124.2(6) . .
C5 N1 Cu1 117.1(5) . .
O1 N2 C9 122.3(7) . .
O1 N2 C9 122.3(7) . 15_454
C9 N2 C9 115.4(14) . 15_454
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
F1 Si1 1.694(12) .
F1 Cu1 2.229(9) .
F2 Si1 1.681(4) .
F3 Si1 1.701(13) .
F3 Cu1 2.224(10) 5_554
C1 N1 1.289(10) .
C1 C2 1.382(11) .
C1 H1 0.9500 .
C2 C3 1.300(13) .
C2 H2 0.9500 .
C3 C4 1.403(13) .
C3 C6 1.526(12) .
C4 C5 1.426(11) .
C4 H4 0.9500 .
C5 N1 1.376(10) .
C5 H5 0.9500 .
C6 C7 1.277(13) .
C6 C8 1.445(15) .
C7 C7 1.452(18) 15_454
C7 H7 0.9500 .
C8 C8 1.411(18) 15_454
C8 C9 1.515(15) .
C9 N2 1.487(14) .
C9 C10 1.520(16) .
C9 C11 1.565(15) .
C10 H10 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C11 H11 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
Cu1 N1 2.022(5) 4
Cu1 N1 2.022(5) 3
Cu1 N1 2.022(5) 2
Cu1 N1 2.022(5) .
Cu1 F3 2.224(10) 5
Si1 F2 1.681(4) 4
Si1 F2 1.681(4) 3
Si1 F2 1.681(4) 2
N2 O1 1.287(19) .
N2 C9 1.487(14) 15_454
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 C1 C2 C3 2.8(17) . .
C1 C2 C3 C4 3.4(17) . .
C1 C2 C3 C6 -177.3(10) . .
C2 C3 C4 C5 -4.7(16) . .
C6 C3 C4 C5 176.0(9) . .
C3 C4 C5 N1 0.3(13) . .
C2 C3 C6 C7 -71.2(16) . .
C4 C3 C6 C7 108.1(12) . .
C2 C3 C6 C8 108.0(13) . .
C4 C3 C6 C8 -72.7(14) . .
C8 C6 C7 C7 -4.1(13) . 15_454
C3 C6 C7 C7 175.1(6) . 15_454
C7 C6 C8 C8 3.9(13) . 15_454
C3 C6 C8 C8 -175.2(7) . 15_454
C7 C6 C8 C9 -179.2(12) . .
C3 C6 C8 C9 1.6(19) . .
C8 C8 C9 N2 1.3(10) 15_454 .
C6 C8 C9 N2 -175.7(13) . .
C8 C8 C9 C10 120.4(9) 15_454 .
C6 C8 C9 C10 -56.6(17) . .
C8 C8 C9 C11 -108.5(8) 15_454 .
C6 C8 C9 C11 74.5(15) . .
Si1 F1 Cu1 N1 0(100) . 4
Si1 F1 Cu1 N1 0(100) . 3
Si1 F1 Cu1 N1 0(100) . 2
Si1 F1 Cu1 N1 0(100) . .
Si1 F1 Cu1 F3 0(100) . 5
Cu1 F1 Si1 F2 0(100) . .
Cu1 F1 Si1 F2 0(100) . 4
Cu1 F1 Si1 F2 0(100) . 3
Cu1 F1 Si1 F2 0(100) . 2
Cu1 F1 Si1 F3 0(100) . .
Cu1 F3 Si1 F2 0(100) 5_554 .
Cu1 F3 Si1 F2 0(100) 5_554 4
Cu1 F3 Si1 F2 0(100) 5_554 3
Cu1 F3 Si1 F2 0(100) 5_554 2
Cu1 F3 Si1 F1 0(100) 5_554 .
C2 C1 N1 C5 -7.2(13) . .
C2 C1 N1 Cu1 171.5(8) . .
C4 C5 N1 C1 5.5(11) . .
C4 C5 N1 Cu1 -173.3(6) . .
N1 Cu1 N1 C1 119.6(6) 4 .
N1 Cu1 N1 C1 -58.6(8) 3 .
N1 Cu1 N1 C1 30.5(7) 2 .
F3 Cu1 N1 C1 -149.5(7) 5 .
F1 Cu1 N1 C1 30.5(7) . .
N1 Cu1 N1 C5 -61.7(7) 4 .
N1 Cu1 N1 C5 120.1(5) 3 .
N1 Cu1 N1 C5 -150.8(5) 2 .
F3 Cu1 N1 C5 29.2(5) 5 .
F1 Cu1 N1 C5 -150.8(5) . .
C8 C9 N2 O1 178.7(17) . .
C10 C9 N2 O1 55(2) . .
C11 C9 N2 O1 -60(2) . .
C8 C9 N2 C9 -2.3(17) . 15_454
C10 C9 N2 C9 -125.5(11) . 15_454
C11 C9 N2 C9 118.7(12) . 15_454
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 0.500 -0.037 1609 177 ' '
2 0.500 0.000 -0.043 1609 177 ' '
