#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/23/7102378.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_7102378
loop_
_publ_author_name
'Maekawa, Masahiko'
'Konaka, Hisashi'
'Minematsu, Toshie'
'Kuroda-Sowa, Takayoshi'
'Munakata, Megumu'
'Kitagawa, Susumu'
_publ_section_title
;
 Bowl-shaped Cu(I) metallamacrocyclic ethylene and carbonyl adducts as
 structural analogues of organic calixarenes.
;
_journal_issue                   48
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5179
_journal_page_last               5181
_journal_paper_doi               10.1039/b713618h
_journal_year                    2007
_chemical_formula_moiety         'C40 H28 Cu4 N12 O4, 4(F6 P)'
_chemical_formula_sum            'C40 H28 Cu4 F24 N12 O4 P4'
_chemical_formula_weight         1574.78
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8455(8)
_cell_length_b                   14.8455(8)
_cell_length_c                   12.2984(9)
_cell_measurement_reflns_used    6379
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2710.4(3)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            15811
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    1.803
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            L
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1552.00
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.40
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3102
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.0291P)²+4.0002P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                2732
_reflns_number_total             3102
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b713618h.txt
_cod_data_source_block           '[Cu4(pprd)4(CO)4](PF6)4_Complex3-CCDC-659370'
_cod_original_sg_symbol_Hall     '-P 4a '
_cod_original_sg_symbol_H-M      'P 4/n '
_cod_original_formula_sum        'C40 H28 Cu4 F24 N12 O4 P4 '
_cod_database_code               7102378
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,z
1/2-y,x,z
y,1/2-x,z
-x,-y,-z
1/2+x,1/2+y,-z
1/2+y,-x,-z
-y,1/2+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
Cu(1) Cu 0.37827(2) -0.00077(2) 0.61783(3) 0.0191(1) Uani 1.00 1 d .
P(1) P 0.7500 0.2500 1.0000 0.0221(3) Uani 1.00 4 d S
P(2) P 0.7500 0.2500 0.5000 0.0226(3) Uani 1.00 4 d S
P(3) P 0.2500 0.2500 0.8802(1) 0.0261(4) Uani 1.00 4 d S
P(4) P 0.2500 0.2500 0.3925(2) 0.0293(4) Uani 1.00 4 d S
F(1) F 0.7500 0.2500 0.8703(2) 0.0320(6) Uani 1.00 2 d S
F(2) F 0.8519(1) 0.2131(1) 0.9995(2) 0.0315(4) Uani 1.00 1 d .
F(3) F 0.7500 0.2500 0.6281(3) 0.073(1) Uani 1.00 2 d S
F(4) F 0.7143(1) 0.3516(1) 0.5005(2) 0.0492(6) Uani 1.00 1 d .
F(5) F 0.2500 0.2500 1.0100(3) 0.0342(9) Uani 1.00 4 d S
F(6) F 0.2045(2) 0.3471(2) 0.8813(2) 0.0594(7) Uani 1.00 1 d .
F(7) F 0.2500 0.2500 0.7511(4) 0.065(1) Uani 1.00 4 d S
F(8) F 0.2500 0.2500 0.5240(4) 0.066(2) Uani 1.00 4 d S
F(9) F 0.3456(2) 0.2032(2) 0.3971(3) 0.084(1) Uani 1.00 1 d .
F(10) F 0.2500 0.2500 0.2682(5) 0.106(3) Uani 1.00 4 d S
O(1) O 0.3566(2) -0.0205(2) 0.3819(2) 0.0343(6) Uani 1.00 1 d .
N(1) N 0.4462(2) 0.1053(2) 0.6865(2) 0.0180(5) Uani 1.00 1 d .
N(2) N 0.4537(2) -0.0681(2) 0.7312(2) 0.0213(5) Uani 1.00 1 d .
N(3) N 0.4963(2) 0.2561(2) 0.6951(2) 0.0185(5) Uani 1.00 1 d .
C(1) C 0.4464(2) 0.1899(2) 0.6527(2) 0.0197(6) Uani 1.00 1 d .
C(2) C 0.5467(2) 0.2342(2) 0.7808(3) 0.0257(7) Uani 1.00 1 d .
C(3) C 0.5492(2) 0.1483(2) 0.8229(3) 0.0268(7) Uani 1.00 1 d .
C(4) C 0.5525(2) -0.0492(2) 0.8827(3) 0.0248(6) Uani 1.00 1 d .
C(5) C 0.5563(2) -0.1418(2) 0.8973(3) 0.0317(8) Uani 1.00 1 d .
C(6) C 0.5080(3) -0.1961(2) 0.8281(3) 0.0355(8) Uani 1.00 1 d .
C(7) C 0.4570(2) -0.1572(2) 0.7467(3) 0.0298(7) Uani 1.00 1 d .
C(8) C 0.4987(2) 0.0830(2) 0.7716(2) 0.0177(6) Uani 1.00 1 d .
C(9) C 0.5013(2) -0.0144(2) 0.7984(2) 0.0189(6) Uani 1.00 1 d .
C(10) C 0.3681(2) -0.0144(2) 0.4717(3) 0.0229(7) Uani 1.00 1 d .
H(1) H 0.5847 -0.0101 0.9300 0.0298 Uiso 1.00 1 calc .
H(2) H 0.5917 -0.1671 0.9540 0.0380 Uiso 1.00 1 calc .
H(3) H 0.5097 -0.2597 0.8362 0.0426 Uiso 1.00 1 calc .
H(4) H 0.5845 0.1345 0.8851 0.0321 Uiso 1.00 1 calc .
H(5) H 0.4080 0.2048 0.5936 0.0237 Uiso 1.00 1 calc .
H(6) H 0.4230 -0.1951 0.6999 0.0358 Uiso 1.00 1 calc .
H(7) H 0.5824 0.2797 0.8141 0.0308 Uiso 1.00 1 calc .
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 6.1.1.4)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
Cu Cu 0.320 1.265
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.102 0.094
;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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N(1) Cu(1) N(2) 79.96(10) . . yes
N(1) Cu(1) N(3) 102.67(10) . 4_555 yes
N(1) Cu(1) C(10) 122.3(1) . . yes
N(2) Cu(1) N(3) 100.60(10) . 4_555 yes
N(2) Cu(1) C(10) 131.7(1) . . yes
N(3) Cu(1) C(10) 112.9(1) 4_555 . yes
F(1) P(1) F(1) 180.0 . 7_567 yes
F(1) P(1) F(2) 89.80(7) . . yes
F(1) P(1) F(2) 90.20(7) . 7_567 yes
F(1) P(1) F(2) 90.20(7) . 8_647 yes
F(1) P(1) F(2) 89.80(7) . 2_655 yes
F(1) P(1) F(2) 90.20(7) 7_567 . yes
F(1) P(1) F(2) 89.80(7) 7_567 7_567 yes
F(1) P(1) F(2) 89.80(7) 7_567 8_647 yes
F(1) P(1) F(2) 90.20(7) 7_567 2_655 yes
F(2) P(1) F(2) 90.001(2) . 7_567 yes
F(2) P(1) F(2) 90.001(2) . 8_647 yes
F(2) P(1) F(2) 179.6(1) . 2_655 yes
F(2) P(1) F(2) 179.6(1) 7_567 8_647 yes
F(2) P(1) F(2) 90.001(2) 7_567 2_655 yes
F(2) P(1) F(2) 90.001(2) 8_647 2_655 yes
F(3) P(2) F(3) 180.0 . 7_566 yes
F(3) P(2) F(4) 89.76(10) . . yes
F(3) P(2) F(4) 90.24(10) . 7_566 yes
F(3) P(2) F(4) 90.24(10) . 8_646 yes
F(3) P(2) F(4) 89.76(10) . 2_655 yes
F(3) P(2) F(4) 90.24(10) 7_566 . yes
F(3) P(2) F(4) 89.76(10) 7_566 7_566 yes
F(3) P(2) F(4) 89.76(10) 7_566 8_646 yes
F(3) P(2) F(4) 90.24(10) 7_566 2_655 yes
F(4) P(2) F(4) 90.001(2) . 7_566 yes
F(4) P(2) F(4) 90.001(2) . 8_646 yes
F(4) P(2) F(4) 179.5(2) . 2_655 yes
F(4) P(2) F(4) 179.5(2) 7_566 8_646 yes
F(4) P(2) F(4) 90.001(2) 7_566 2_655 yes
F(4) P(2) F(4) 90.001(2) 8_646 2_655 yes
F(5) P(3) F(6) 89.5(1) . . yes
F(5) P(3) F(6) 89.5(1) . 2_555 yes
F(5) P(3) F(6) 89.5(1) . 3_555 yes
F(5) P(3) F(6) 89.5(1) . 4_555 yes
F(5) P(3) F(7) 180.0 . . yes
F(6) P(3) F(6) 179.0(2) . 2_555 yes
F(6) P(3) F(6) 89.996(3) . 3_555 yes
F(6) P(3) F(6) 89.996(3) . 4_555 yes
F(6) P(3) F(7) 90.5(1) . . yes
F(6) P(3) F(6) 89.996(3) 2_555 3_555 yes
F(6) P(3) F(6) 89.996(3) 2_555 4_555 yes
F(6) P(3) F(7) 90.5(1) 2_555 . yes
F(6) P(3) F(6) 179.0(2) 3_555 4_555 yes
F(6) P(3) F(7) 90.5(1) 3_555 . yes
F(6) P(3) F(7) 90.5(1) 4_555 . yes
F(8) P(4) F(9) 87.9(1) . . yes
F(8) P(4) F(9) 87.9(1) . 2_555 yes
F(8) P(4) F(9) 87.9(1) . 3_555 yes
F(8) P(4) F(9) 87.9(1) . 4_555 yes
F(8) P(4) F(10) 180.0 . . yes
F(9) P(4) F(9) 175.9(3) . 2_555 yes
F(9) P(4) F(9) 89.93(1) . 3_555 yes
F(9) P(4) F(9) 89.93(1) . 4_555 yes
F(9) P(4) F(10) 92.1(1) . . yes
F(9) P(4) F(9) 89.93(1) 2_555 3_555 yes
F(9) P(4) F(9) 89.93(1) 2_555 4_555 yes
F(9) P(4) F(10) 92.1(1) 2_555 . yes
F(9) P(4) F(9) 175.9(3) 3_555 4_555 yes
F(9) P(4) F(10) 92.1(1) 3_555 . yes
F(9) P(4) F(10) 92.1(1) 4_555 . yes
Cu(1) N(1) C(1) 126.9(2) . . yes
Cu(1) N(1) C(8) 114.6(2) . . yes
C(1) N(1) C(8) 118.4(3) . . yes
Cu(1) N(2) C(7) 126.8(2) . . yes
Cu(1) N(2) C(9) 114.5(2) . . yes
C(7) N(2) C(9) 118.6(3) . . yes
Cu(1) N(3) C(1) 119.3(2) 3_555 . yes
Cu(1) N(3) C(2) 124.3(2) 3_555 . yes
C(1) N(3) C(2) 116.1(3) . . yes
N(1) C(1) N(3) 125.3(3) . . yes
N(1) C(1) H(5) 117.4 . . no
N(3) C(1) H(5) 117.4 . . no
N(3) C(2) C(3) 122.5(3) . . yes
N(3) C(2) H(7) 118.7 . . no
C(3) C(2) H(7) 118.7 . . no
C(2) C(3) C(8) 117.7(3) . . yes
C(2) C(3) H(4) 121.1 . . no
C(8) C(3) H(4) 121.1 . . no
C(5) C(4) C(9) 119.3(3) . . yes
C(5) C(4) H(1) 120.4 . . no
C(9) C(4) H(1) 120.4 . . no
C(4) C(5) C(6) 118.7(3) . . yes
C(4) C(5) H(2) 120.7 . . no
C(6) C(5) H(2) 120.7 . . no
C(5) C(6) C(7) 119.3(3) . . yes
C(5) C(6) H(3) 120.3 . . no
C(7) C(6) H(3) 120.3 . . no
N(2) C(7) C(6) 122.4(3) . . yes
N(2) C(7) H(6) 118.8 . . no
C(6) C(7) H(6) 118.8 . . no
N(1) C(8) C(3) 119.8(3) . . yes
N(1) C(8) C(9) 115.4(2) . . yes
C(3) C(8) C(9) 124.7(3) . . yes
N(2) C(9) C(4) 121.7(3) . . yes
N(2) C(9) C(8) 115.2(3) . . yes
C(4) C(9) C(8) 123.0(3) . . yes
Cu(1) C(10) O(1) 175.6(3) . . 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) N(1) 2.051(2) . yes
Cu(1) N(2) 2.048(3) . yes
Cu(1) N(3) 2.048(2) 4_555 yes
Cu(1) C(10) 1.815(3) . yes
P(1) F(1) 1.596(3) . yes
P(1) F(1) 1.596(3) 7_567 yes
P(1) F(2) 1.610(2) . yes
P(1) F(2) 1.610(2) 7_567 yes
P(1) F(2) 1.610(2) 8_647 yes
P(1) F(2) 1.610(2) 2_655 yes
P(2) F(3) 1.575(3) . yes
P(2) F(3) 1.575(3) 7_566 yes
P(2) F(4) 1.598(2) . yes
P(2) F(4) 1.598(2) 7_566 yes
P(2) F(4) 1.598(2) 8_646 yes
P(2) F(4) 1.598(2) 2_655 yes
P(3) F(5) 1.596(4) . yes
P(3) F(6) 1.592(3) . yes
P(3) F(6) 1.592(3) 2_555 yes
P(3) F(6) 1.592(3) 3_555 yes
P(3) F(6) 1.592(3) 4_555 yes
P(3) F(7) 1.587(5) . yes
P(4) F(8) 1.618(5) . yes
P(4) F(9) 1.581(3) . yes
P(4) F(9) 1.581(3) 2_555 yes
P(4) F(9) 1.581(3) 3_555 yes
P(4) F(9) 1.581(3) 4_555 yes
P(4) F(10) 1.529(6) . yes
O(1) C(10) 1.121(4) . yes
N(1) C(1) 1.323(4) . yes
N(1) C(8) 1.346(4) . yes
N(2) C(7) 1.337(4) . yes
N(2) C(9) 1.349(4) . yes
N(3) C(1) 1.337(4) . yes
N(3) C(2) 1.334(4) . yes
C(1) H(5) 0.950 . no
C(2) C(3) 1.378(4) . yes
C(2) H(7) 0.950 . no
C(3) C(8) 1.379(4) . yes
C(3) H(4) 0.950 . no
C(4) C(5) 1.387(5) . yes
C(4) C(9) 1.385(4) . yes
C(4) H(1) 0.950 . no
C(5) C(6) 1.374(5) . yes
C(5) H(2) 0.950 . no
C(6) C(7) 1.383(5) . yes
C(6) H(3) 0.950 . no
C(7) H(6) 0.950 . no
C(8) C(9) 1.483(4) . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Cu(1) F(4) 3.585(2) 6_446
F(2) C(6) 3.418(4) 6_557
F(4) C(10) 3.048(4) 6_556
F(4) O(1) 3.187(3) 6_556
F(5) F(10) 3.175(7) 1_556
F(5) C(5) 3.485(4) 5_657
F(5) C(5) 3.485(4) 6_457
F(5) C(5) 3.485(4) 8_547
F(6) C(5) 3.504(4) 6_457
F(9) C(7) 3.491(5) 5_656
F(9) C(6) 3.522(5) 5_656
O(1) C(8) 3.007(4) 5_656
O(1) C(9) 3.105(4) 5_656
O(1) N(1) 3.296(3) 5_656
O(1) C(7) 3.373(4) 8_546
O(1) N(2) 3.406(3) 5_656
O(1) C(3) 3.450(4) 5_656
O(1) C(6) 3.540(4) 8_546
C(4) C(4) 3.590(6) 5_657
