#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/46/4114676.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_4114676
loop_
_publ_author_name
'Shin-ichiro Noro'
'Ryo Kitaura'
'Mitsuru Kondo'
'Susumu Kitagawa'
'Tomohiko Ishii'
'Hiroyuki Matsuzaka'
'Masahiro Yamashita'
_publ_section_title
;
 Framework Engineering by Anions and Porous Functionalities of
 Cu(II)/4,4'-bpy Coordination Polymers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2568
_journal_page_last               2583
_journal_paper_doi               10.1021/ja0113192
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C20 H26 Cu F6 N4 O5 Si'
_chemical_formula_weight         608.07
_space_group_IT_number           123
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      123
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.0449(6)
_cell_length_b                   11.0449(6)
_cell_length_c                   8.055(1)
_cell_measurement_reflns_used    11566
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.8
_cell_volume                     982.63(14)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9986
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.116
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5088
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_exptl_absorpt_coefficient_mu    6.40
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            pale-purple
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_description       block
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.27
_refine_diff_density_min         -1.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.891
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     44
_refine_ls_number_reflns         447
_refine_ls_R_factor_gt           0.1287
_refine_ls_shift/su_max          2.3688
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00010|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                447
_reflns_number_total             716
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja0113192_8.cif
_cod_data_source_block           {[Cu(SiF6)(4,4'-bpy)2].5H2O}n
_cod_original_cell_volume        982.6(1)
_cod_original_formula_sum        'C20 H26 Cu F6 N4 O5 Si '
_cod_database_code               4114676
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
-x,y,z
x,-y,z
-y,x,z
y,-x,z
y,x,z
-y,-x,z
-x,-y,-z
x,y,-z
x,-y,-z
-x,y,-z
y,-x,-z
-y,x,-z
-y,-x,-z
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_calc_flag
_atom_site_refinement_flags
Cu(1) Cu 0.5000 0.5000 1.0000 0.0392(10) Uani 1.00 d S
Si(1) Si 0.5000 0.5000 0.5000 0.052(2) Uani 1.00 d S
F(1) F 0.5000 0.5000 0.290(2) 0.050(3) Uani 1.00 d S
F(2) F 0.3921(7) 0.3921 0.5000 0.102(3) Uani 1.00 d S
O(1) O 1.0000 0.0000 0.5000 0.49(3) Uani 1.00 d S
O(2) O 1.362(8) 0.0000 0.5000 0.82(8) Uani 1.00 d S
N(1) N 0.5000 0.322(2) 1.0000 0.057(5) Uani 1.00 d S
C(1) C 0.453(2) 0.258(2) 1.123(3) 0.11(1) Uani 0.50 d P
C(2) C 0.450(3) 0.136(2) 1.134(2) 0.12(1) Uani 0.50 d P
C(3) C 0.5000 0.072(2) 1.0000 0.064(7) Uani 1.00 d S
H(1) H 0.4187 0.3022 1.2129 0.1238 Uiso 0.50 calc P
H(2) H 0.4135 0.0977 1.2260 0.1361 Uiso 0.50 calc P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cu Cu 0.320 1.265
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Si Si 0.082 0.070
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
F F 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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
F(1) Cu(1) F(1) 180.0 1_556 9_666 yes
F(1) Cu(1) N(1) 90.0 1_556 . yes
F(1) Cu(1) N(1) 90.0 1_556 6_565 yes
F(1) Cu(1) N(1) 90.0 1_556 5_655 yes
F(1) Cu(1) N(1) 90.0 1_556 2_665 yes
F(1) Cu(1) N(1) 90.0 9_666 . yes
F(1) Cu(1) N(1) 90.0 9_666 6_565 yes
F(1) Cu(1) N(1) 90.0 9_666 5_655 yes
F(1) Cu(1) N(1) 90.0 9_666 2_665 yes
N(1) Cu(1) N(1) 90.0 . 6_565 yes
N(1) Cu(1) N(1) 90.0 . 5_655 yes
N(1) Cu(1) N(1) 180.0 . 2_665 yes
N(1) Cu(1) N(1) 180.0 6_565 5_655 yes
N(1) Cu(1) N(1) 90.0 6_565 2_665 yes
N(1) Cu(1) N(1) 90.0 5_655 2_665 yes
F(1) Si(1) F(1) 180.0 . 9_666 yes
F(1) Si(1) F(2) 90.0 . . yes
F(1) Si(1) F(2) 90.0 . 4_565 yes
F(1) Si(1) F(2) 90.0 . 3_655 yes
F(1) Si(1) F(2) 90.0 . 2_665 yes
F(1) Si(1) F(2) 90.0 9_666 . yes
F(1) Si(1) F(2) 90.0 9_666 4_565 yes
F(1) Si(1) F(2) 90.0 9_666 3_655 yes
F(1) Si(1) F(2) 90.0 9_666 2_665 yes
F(2) Si(1) F(2) 90.000(3) . 4_565 yes
F(2) Si(1) F(2) 90.000(3) . 3_655 yes
F(2) Si(1) F(2) 180.0 . 2_665 yes
F(2) Si(1) F(2) 180.0 4_565 3_655 yes
F(2) Si(1) F(2) 90.000(3) 4_565 2_665 yes
F(2) Si(1) F(2) 90.000(3) 3_655 2_665 yes
Cu(1) F(1) Si(1) 180.0000(1) 1_554 . yes
Cu(1) N(1) C(1) 122(1) . . yes
Cu(1) N(1) C(1) 122(1) . 10_557 yes
Cu(1) N(1) C(1) 122(1) . 3_655 yes
Cu(1) N(1) C(1) 122(1) . 12_657 yes
C(1) N(1) C(1) 96(2) . 10_557 yes
C(1) N(1) C(1) 46(2) . 3_655 yes
C(1) N(1) C(1) 115(2) . 12_657 yes
C(1) N(1) C(1) 115(2) 10_557 3_655 yes
C(1) N(1) C(1) 46(2) 10_557 12_657 yes
C(1) N(1) C(1) 96(2) 3_655 12_657 yes
N(1) C(1) C(1) 41(1) . 10_557 yes
N(1) C(1) C(1) 66(1) . 3_655 yes
N(1) C(1) C(1) 32(1) . 12_657 yes
N(1) C(1) C(2) 126(2) . . yes
N(1) C(1) C(2) 102(2) . 3_655 yes
N(1) C(1) C(3) 94(1) . . yes
C(1) C(1) C(1) 90.0 10_557 3_655 yes
C(1) C(1) C(1) 27(1) 10_557 12_657 yes
C(1) C(1) C(2) 93(1) 10_557 . yes
C(1) C(1) C(2) 93(1) 10_557 3_655 yes
C(1) C(1) C(3) 65.0(5) 10_557 . yes
C(1) C(1) C(1) 62(1) 3_655 12_657 yes
C(1) C(1) C(2) 91(1) 3_655 . yes
C(1) C(1) C(2) 51(1) 3_655 3_655 yes
C(1) C(1) C(3) 77.2(7) 3_655 . yes
C(1) C(1) C(2) 93(1) 12_657 . yes
C(1) C(1) C(2) 76(1) 12_657 3_655 yes
C(1) C(1) C(3) 61.5(5) 12_657 . yes
C(2) C(1) C(2) 39(2) . 3_655 yes
C(2) C(1) C(3) 32(1) . . yes
C(2) C(1) C(3) 36.6(10) 3_655 . yes
C(1) C(2) C(1) 37(2) . 3_655 yes
C(1) C(2) C(2) 86(1) . 10_557 yes
C(1) C(2) C(2) 88(1) . 3_655 yes
C(1) C(2) C(3) 116(2) . . yes
C(1) C(2) C(2) 86(1) 3_655 10_557 yes
C(1) C(2) C(2) 51(1) 3_655 3_655 yes
C(1) C(2) C(3) 96(2) 3_655 . yes
C(2) C(2) C(2) 90.0 10_557 3_655 yes
C(2) C(2) C(3) 39(1) 10_557 . yes
C(2) C(2) C(3) 67(1) 3_655 . yes
C(1) C(3) C(1) 49(1) . 10_557 yes
C(1) C(3) C(1) 25(1) . 3_655 yes
C(1) C(3) C(1) 56(1) . 12_657 yes
C(1) C(3) C(2) 30(1) . . yes
C(1) C(3) C(2) 77(1) . 10_557 yes
C(1) C(3) C(2) 46(1) . 3_655 yes
C(1) C(3) C(2) 87(1) . 12_657 yes
C(1) C(3) C(3) 151.5(5) . 2_655 yes
C(1) C(3) C(1) 56(1) 10_557 3_655 yes
C(1) C(3) C(1) 25(1) 10_557 12_657 yes
C(1) C(3) C(2) 77(1) 10_557 . yes
C(1) C(3) C(2) 30(1) 10_557 10_557 yes
C(1) C(3) C(2) 87(1) 10_557 3_655 yes
C(1) C(3) C(2) 46(1) 10_557 12_657 yes
C(1) C(3) C(3) 151.5(5) 10_557 2_655 yes
C(1) C(3) C(1) 49(1) 3_655 12_657 yes
C(1) C(3) C(2) 46(1) 3_655 . yes
C(1) C(3) C(2) 87(1) 3_655 10_557 yes
C(1) C(3) C(2) 30(1) 3_655 3_655 yes
C(1) C(3) C(2) 77(1) 3_655 12_657 yes
C(1) C(3) C(3) 151.5(5) 3_655 2_655 yes
C(1) C(3) C(2) 87(1) 12_657 . yes
C(1) C(3) C(2) 46(1) 12_657 10_557 yes
C(1) C(3) C(2) 77(1) 12_657 3_655 yes
C(1) C(3) C(2) 30(1) 12_657 12_657 yes
C(1) C(3) C(3) 151.5(5) 12_657 2_655 yes
C(2) C(3) C(2) 100(2) . 10_557 yes
C(2) C(3) C(2) 45(2) . 3_655 yes
C(2) C(3) C(2) 118(2) . 12_657 yes
C(2) C(3) C(3) 120(1) . 2_655 yes
C(2) C(3) C(2) 118(2) 10_557 3_655 yes
C(2) C(3) C(2) 45(2) 10_557 12_657 yes
C(2) C(3) C(3) 120(1) 10_557 2_655 yes
C(2) C(3) C(2) 100(2) 3_655 12_657 yes
C(2) C(3) C(3) 120(1) 3_655 2_655 yes
C(2) C(3) C(3) 120(1) 12_657 2_655 yes
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
Cu(1) F(1) 2.34(1) 1_556 yes
Cu(1) F(1) 2.34(1) 9_666 yes
Cu(1) N(1) 1.96(2) . yes
Cu(1) N(1) 1.96(2) 6_565 yes
Cu(1) N(1) 1.96(2) 5_655 yes
Cu(1) N(1) 1.96(2) 2_665 yes
Si(1) F(1) 1.69(1) . yes
Si(1) F(1) 1.69(1) 9_666 yes
Si(1) F(2) 1.69(1) . yes
Si(1) F(2) 1.69(1) 4_565 yes
Si(1) F(2) 1.69(1) 3_655 yes
Si(1) F(2) 1.69(1) 2_665 yes
N(1) C(1) 1.32(2) . yes
N(1) C(1) 1.32(2) 10_557 yes
N(1) C(1) 1.32(2) 3_655 yes
N(1) C(1) 1.32(2) 12_657 yes
C(1) C(1) 1.98(4) 10_557 yes
C(1) C(1) 1.04(6) 3_655 yes
C(1) C(1) 2.23(4) 12_657 yes
C(1) C(2) 1.35(3) . yes
C(1) C(2) 1.72(3) 3_655 yes
C(1) C(3) 2.34(3) . yes
C(2) C(2) 2.16(4) 10_557 yes
C(2) C(2) 1.10(6) 3_655 yes
C(2) C(3) 1.41(2) . yes
C(3) C(3) 1.58(4) 2_655 yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Cu(1) C(1) 2.90(2) 4_565
Cu(1) C(1) 2.90(2) 7_555
Cu(1) C(1) 2.90(2) 8_665
Cu(1) C(1) 2.90(2) 9_667
Cu(1) C(1) 2.90(2) 11_567
Cu(1) C(1) 2.90(2) 13_567
Cu(1) C(1) 2.90(2) 14_657
Cu(1) C(1) 2.90(2) 15_667
Cu(1) C(1) 2.90(2) 16_557
F(1) C(1) 3.04(2) 1_554
F(1) C(1) 3.04(2) 2_664
F(1) C(1) 3.04(2) 3_654
F(1) C(1) 3.04(2) 4_564
F(1) C(1) 3.04(2) 5_654
F(1) C(1) 3.04(2) 6_564
F(1) C(1) 3.04(2) 7_554
F(1) C(1) 3.04(2) 8_664
F(1) N(1) 3.05(2) 1_554
F(1) N(1) 3.05(2) 2_664
F(1) N(1) 3.05(2) 5_654
F(1) N(1) 3.05(2) 6_564
O(2) O(2) 3.0(2) 2_855
N(1) C(1) 3.19(2) 7_555
N(1) C(1) 3.19(2) 14_657
N(1) C(1) 3.19(2) 16_557
C(1) C(1) 3.05(5) 7_555
C(2) C(2) 3.01(5) 4_555
