#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:30:11 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179922 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/17/7021757.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_7021757
loop_
_publ_author_name
'Noro, Shin-Ichiro'
'Fukuhara, Katsuo'
'Sugimoto, Kunihisa'
'Hijikata, Yuh'
'Kubo, Kazuya'
'Nakamura, Takayoshi'
_publ_section_title
;
 Anion-dependent host-guest properties of porous assemblies of
 coordination complexes (PACs), [Cu(A)2(py)4] (A = PF6, BF4, CF3SO3, and
 CH3SO3; py = pyridine), based on Werner-type copper(ii) complexes in the
 solid state.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11100
_journal_page_last               11110
_journal_paper_doi               10.1039/c3dt51104a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C30 H30 Cu F12 N6 P2'
_chemical_formula_sum            'C30 H30 Cu F12 N6 P2'
_chemical_formula_weight         828.08
_space_group_IT_number           97
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      97
_symmetry_space_group_name_Hall  'I 4 2'
_symmetry_space_group_name_H-M   'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   11.2091(7)
_cell_length_b                   11.2091(7)
_cell_length_c                   13.9590(11)
_cell_measurement_reflns_used    6699
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      3.63
_cell_volume                     1753.9(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6982
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             838.00
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.230
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  399 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.024(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     63
_refine_ls_number_reflns         1013
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0531P)²+0.0821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                961
_reflns_number_total             1013
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c3dt51104a.txt
_cod_data_source_block           b-CuPF6py_py_111008
_cod_database_code               7021757
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -Y,+X,+Z
3 -X,-Y,+Z
4 +Y,-X,+Z
5 -X,+Y,-Z
6 +Y,+X,-Z
7 +X,-Y,-Z
8 -Y,-X,-Z
9 1/2+X,1/2+Y,1/2+Z
10 1/2-Y,1/2+X,1/2+Z
11 1/2-X,1/2-Y,1/2+Z
12 1/2+Y,1/2-X,1/2+Z
13 1/2-X,1/2+Y,1/2-Z
14 1/2+Y,1/2+X,1/2-Z
15 1/2+X,1/2-Y,1/2-Z
16 1/2-Y,1/2-X,1/2-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 1.0000 1.0000 0.5000 0.02308(16) Uani 1.0 2 d .
P1 P 1.0000 1.0000 0.78961(5) 0.0274(2) Uani 1.0 4 d .
F1 F 1.0000 1.0000 0.67325(15) 0.0415(5) Uani 1.0 4 d .
F2 F 1.0000 1.0000 0.90392(15) 0.0580(7) Uani 1.0 4 d .
F3 F 1.02011(16) 0.85974(11) 0.78820(10) 0.0596(5) Uani 1.0 16 d .
N1 N 0.87227(10) 0.87227(10) 0.5000 0.0272(4) Uani 1.0 8 d .
C1 C 0.86745(18) 0.78983(17) 0.56996(15) 0.0359(4) Uani 1.0 16 d .
C2 C 0.7802(2) 0.70258(19) 0.5725(2) 0.0470(5) Uani 1.0 16 d .
C3 C 0.69706(14) 0.69706(14) 0.5000 0.0496(7) Uani 1.0 8 d .
C4 C 1.0832(3) 0.4168(3) 0.2500 0.108(3) Uani 1.0 8 d .
C5 C 1.0423(5) 0.4587(5) 0.1652(5) 0.1263(19) Uani 1.0 16 d .
H1 H 0.9259 0.7916 0.6192 0.0431 Uiso 1.0 16 calc R
H2 H 0.7777 0.6470 0.6238 0.0563 Uiso 1.0 16 calc R
H3 H 0.6371 0.6371 0.5000 0.0596 Uiso 1.0 8 calc R
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 for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(1992, 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
F1 Cu1 F1 180.000 yes . 5_756
F1 Cu1 N1 90.000 yes . .
F1 Cu1 N1 90.000 yes . 2_755
F1 Cu1 N1 90.000 yes . 3_775
F1 Cu1 N1 90.000 yes . 4_575
F1 Cu1 N1 90.000 yes 5_756 .
F1 Cu1 N1 90.000 yes 5_756 2_755
F1 Cu1 N1 90.000 yes 5_756 3_775
F1 Cu1 N1 90.000 yes 5_756 4_575
N1 Cu1 N1 90.00(5) yes . 2_755
N1 Cu1 N1 180.00(5) yes . 3_775
N1 Cu1 N1 90.00(5) yes . 4_575
N1 Cu1 N1 90.00(5) yes 2_755 3_775
N1 Cu1 N1 180.00(5) yes 2_755 4_575
N1 Cu1 N1 90.00(5) yes 3_775 4_575
F1 P1 F2 180.000 yes . .
F1 P1 F3 89.29(6) yes . .
F1 P1 F3 89.29(6) yes . 2_755
F1 P1 F3 89.29(6) yes . 3_775
F1 P1 F3 89.29(6) yes . 4_575
F2 P1 F3 90.71(6) yes . .
F2 P1 F3 90.71(6) yes . 2_755
F2 P1 F3 90.71(6) yes . 3_775
F2 P1 F3 90.71(6) yes . 4_575
F3 P1 F3 89.99(9) yes . 2_755
F3 P1 F3 178.58(9) yes . 3_775
F3 P1 F3 89.99(9) yes . 4_575
F3 P1 F3 89.99(9) yes 2_755 3_775
F3 P1 F3 178.58(9) yes 2_755 4_575
F3 P1 F3 89.99(9) yes 3_775 4_575
Cu1 F1 P1 180.000 yes . .
Cu1 N1 C1 120.93(10) yes . .
Cu1 N1 C1 120.93(10) yes . 6_556
C1 N1 C1 118.14(15) yes . 6_556
N1 C1 C2 122.2(2) yes . .
C1 C2 C3 119.4(2) yes . .
C2 C3 C2 118.62(18) yes . 6_556
C5 C4 C5 122.0(4) yes . 16_665
C4 C5 C5 119.0(6) yes . 3_765
N1 C1 H1 118.926 no . .
C2 C1 H1 118.912 no . .
C1 C2 H2 120.279 no . .
C3 C2 H2 120.281 no . .
C2 C3 H3 120.689 no . .
C2 C3 H3 120.689 no 6_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Cu1 F1 2.418(2) yes .
Cu1 F1 2.418(2) yes 5_756
Cu1 N1 2.0248(12) yes .
Cu1 N1 2.0248(12) yes 2_755
Cu1 N1 2.0248(12) yes 3_775
Cu1 N1 2.0248(12) yes 4_575
P1 F1 1.624(3) yes .
P1 F2 1.596(3) yes .
P1 F3 1.5884(13) yes .
P1 F3 1.5884(13) yes 2_755
P1 F3 1.5884(13) yes 3_775
P1 F3 1.5884(13) yes 4_575
N1 C1 1.346(3) yes .
N1 C1 1.346(3) yes 6_556
C1 C2 1.383(3) yes .
C2 C3 1.377(3) yes .
C4 C5 1.353(7) yes .
C4 C5 1.353(7) yes 16_665
C5 C5 1.325(8) yes 3_765
C1 H1 0.950 no .
C2 H2 0.950 no .
C3 H3 0.950 no .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_2
N1 C2 2.389(3) no 6_556
N1 C3 2.777(2) no .
C1 C2 2.717(4) no 6_556
C4 C4 2.638(5) no 3_765
Cu1 C1 2.951(2) no 7_576
Cu1 C1 2.951(2) no 8_776
F2 F2 2.682(3) no 5_757
F2 C3 3.3995(17) no 9_555
F2 C3 3.3995(17) no 10_655
F2 C3 3.3995(17) no 11_665
F2 C3 3.3995(17) no 12_565
F3 C2 3.574(3) no 15_566
F3 C2 3.532(3) no 16_666
F3 C4 3.224(4) no 7_566
C2 F3 3.574(3) no 15_466
C2 F3 3.532(3) no 16_666
C3 F2 3.3995(17) no 9_444
C3 F2 3.3995(17) no 13_646
C4 F3 3.224(4) no 7_566
C4 F3 3.224(4) no 12_564
C4 C5 2.308(7) no 14_545
C5 C5 2.712(9) no 14_545
F1 H1 2.5915 no .
F1 H1 2.5915 no 2_755
F1 H1 2.5915 no 3_775
F1 H1 2.5915 no 4_575
F3 H1 2.6947 no .
N1 H1 1.9874 no 6_556
C3 H2 2.0292 no 6_556
H1 H2 2.3219 no .
H2 H3 2.3409 no .
Cu1 H1 2.9864 no 7_576
Cu1 H1 2.9864 no 8_776
F2 H2 3.5428 no 13_656
F2 H2 3.5428 no 14_556
F2 H2 3.5428 no 15_566
F2 H2 3.5428 no 16_666
F2 H3 2.5542 no 9_555
F2 H3 2.5542 no 10_655
F2 H3 2.5542 no 11_665
F2 H3 2.5542 no 12_565
F3 H2 3.1387 no 15_566
F3 H2 2.7183 no 16_666
F3 H3 3.4422 no 11_665
F3 H3 3.2346 no 12_565
C4 H1 3.4493 no 7_566
C4 H1 3.4493 no 12_564
C4 H2 3.4915 no 5_756
C4 H2 3.4915 no 10_644
C5 H1 3.1461 no 12_564
C5 H2 2.9913 no 10_644
C5 H2 3.2320 no 12_564
H1 C4 3.4493 no 7_566
H1 C5 3.1461 no 10_645
H2 F2 3.5428 no 13_646
H2 F3 3.1387 no 15_466
H2 F3 2.7183 no 16_666
H2 C4 3.4915 no 5_756
H2 C5 3.2320 no 10_645
H2 C5 2.9913 no 12_565
H3 F2 2.5542 no 9_444
H3 F2 2.5542 no 13_646
H3 F3 3.2346 no 10_644
H3 F3 3.4422 no 11_664
H3 F3 3.2346 no 15_466
H3 F3 3.4422 no 16_666
H3 H3 3.0742 no 2_655
H3 H3 3.0742 no 4_565
