#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:32:27 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180477 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/46/7214646.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_7214646
loop_
_publ_author_name
'Maekawa, Masahiko'
'Tominaga, Toshi'
'Sugimoto, Kunihisa'
'Okubo, Takashi'
'Kuroda--Sowa, Takayoshi'
'Munakata, Megumu'
'Kitagawa, Susumu'
_publ_section_title
;
 Structural controls of 2D sheet copper(i) ethylene and carbonyl
 coordination polymers directed by anions and solvents
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              5955
_journal_paper_doi               10.1039/c2ce25211b
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C37 H30 Cu4 F24 N14 O3 P4'
_chemical_formula_weight         1552.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-12-13T20:40:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.3797(15)
_cell_length_b                   14.3797(15)
_cell_length_c                   23.083(3)
_cell_measurement_temperature    120(2)
_cell_volume                     4133.5(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10806
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    1.772
_exptl_absorpt_correction_T_max  0.9166
_exptl_absorpt_correction_T_min  0.7183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2298
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0533P)²+30.4239P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                3882
_reflns_number_total             4212
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2ce25211b.txt
_cod_data_source_block           {[Cu4(Me2bpm)3(CO)3(MeCN)](PF6)4_0.33MeCN}n
_cod_original_cell_volume        4133.6(8)
_cod_database_code               7214646
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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 0 0.29539(5) 0.0135(2) Uani 1 3 d S
Cu2 Cu 0.38958(5) 0.20108(5) 0.14569(3) 0.01305(15) Uani 1 1 d .
P1 P 0.15836(14) 0.32551(15) 0.09180(9) 0.0321(4) Uani 1 1 d .
P2 P 0.3333 0.6667 0.32383(11) 0.0209(5) Uani 1 3 d S
F1A F 0.1966(8) 0.4328(9) 0.0555(5) 0.0549(16) Uani 0.592(13) 1 d P
F2A F 0.1193(9) 0.2413(10) 0.1427(5) 0.0549(16) Uani 0.592(13) 1 d P
F3A F 0.0389(7) 0.3109(9) 0.0895(4) 0.0549(16) Uani 0.592(13) 1 d P
F4A F 0.1434(8) 0.2614(8) 0.0353(4) 0.0549(16) Uani 0.592(13) 1 d P
F5A F 0.2795(10) 0.3514(9) 0.0976(6) 0.0549(16) Uani 0.592(13) 1 d P
F6A F 0.1745(7) 0.3925(8) 0.1525(5) 0.0549(16) Uani 0.592(13) 1 d P
F1B F 0.1856(12) 0.4015(12) 0.0349(7) 0.057(2) Uani 0.408(13) 1 d P
F2B F 0.1331(13) 0.2181(13) 0.1296(7) 0.057(2) Uani 0.408(13) 1 d P
F3B F 0.0339(11) 0.2521(12) 0.0747(6) 0.057(2) Uani 0.408(13) 1 d P
F4B F 0.1760(12) 0.2445(11) 0.0490(6) 0.057(2) Uani 0.408(13) 1 d P
F5B F 0.2806(15) 0.3795(13) 0.1055(9) 0.057(2) Uani 0.408(13) 1 d P
F6B F 0.1467(11) 0.4063(11) 0.1289(7) 0.057(2) Uani 0.408(13) 1 d P
F7 F 0.2688(5) 0.7023(5) 0.2846(2) 0.0647(16) Uani 1 1 d .
F8 F 0.3690(6) 0.7688(4) 0.3644(2) 0.0777(19) Uani 1 1 d .
N1 N 0.2913(4) 0.0901(4) 0.2066(2) 0.0140(9) Uani 1 1 d .
N2 N 0.1330(3) -0.0037(3) 0.26529(19) 0.0125(9) Uani 1 1 d .
N3 N 0.4852(3) 0.1353(4) 0.17034(19) 0.0134(9) Uani 1 1 d .
N4 N 0.6418(4) 0.1200(4) 0.1743(2) 0.0149(9) Uani 1 1 d .
N6 N 0.6667 0.3333 0.2558(7) 0.078(5) Uani 1 3 d S
C1 C 0.1915(4) 0.0672(4) 0.2242(2) 0.0130(10) Uani 1 1 d .
H1 H 0.161 0.1047 0.2057 0.016 Uiso 1 1 calc R
C2 C 0.1740(4) -0.0604(4) 0.2903(2) 0.0133(10) Uani 1 1 d .
C3 C 0.2728(5) -0.0465(4) 0.2725(2) 0.0178(11) Uani 1 1 d .
H3 H 0.3002 -0.0888 0.2886 0.021 Uiso 1 1 calc R
C4 C 0.3303(4) 0.0304(4) 0.2306(2) 0.0119(10) Uani 1 1 d .
C5 C 0.1128(4) -0.1366(4) 0.3388(3) 0.0166(11) Uani 1 1 d .
H5A H 0.0357 -0.1725 0.3304 0.025 Uiso 1 1 calc R
H5B H 0.1276 -0.0966 0.3752 0.025 Uiso 1 1 calc R
H5C H 0.1353 -0.1905 0.3423 0.025 Uiso 1 1 calc R
C6 C 0.5831(4) 0.1616(4) 0.1546(2) 0.0168(11) Uani 1 1 d .
H6 H 0.6157 0.2163 0.126 0.02 Uiso 1 1 calc R
C7 C 0.5941(4) 0.0374(4) 0.2119(2) 0.0160(11) Uani 1 1 d .
C8 C 0.4874(4) 0.0012(4) 0.2293(3) 0.0168(11) Uani 1 1 d .
H8 H 0.451 -0.0593 0.2541 0.02 Uiso 1 1 calc R
C9 C 0.4376(5) 0.0545(4) 0.2102(2) 0.0153(11) Uani 1 1 d .
C10 C 0.6555(5) -0.0105(5) 0.2364(3) 0.0237(13) Uani 1 1 d .
H10A H 0.6959 -0.0212 0.2055 0.036 Uiso 1 1 calc R
H10B H 0.6058 -0.0799 0.2542 0.036 Uiso 1 1 calc R
H10C H 0.7054 0.0377 0.2658 0.036 Uiso 1 1 calc R
O1 O 0.3099(5) 0.1777(5) 0.0258(2) 0.0476(12) Uani 1 1 d .
C11 C 0.3403(8) 0.1867(7) 0.0717(3) 0.0476(12) Uani 1 1 d .
N5 N 0 0 0.3797(4) 0.0378(16) Uani 1 3 d S
C12 C 0 0 0.4292(5) 0.0378(16) Uani 1 3 d S
C13 C 0 0 0.4913(5) 0.0378(16) Uani 1 3 d S
H13A H 0.0302 -0.0436 0.5054 0.057 Uiso 0.33 1 calc PR
H13B H -0.0738 -0.0302 0.5054 0.057 Uiso 0.33 1 calc PR
H13C H 0.0436 0.0738 0.5054 0.057 Uiso 0.33 1 calc PR
C14 C 0.6667 0.3333 0.3035(8) 0.067(5) Uani 1 3 d S
C15 C 0.6667 0.3333 0.3665(8) 0.071(5) Uani 1 3 d S
H15A H 0.7081 0.3008 0.3806 0.107 Uiso 0.33 1 calc PR
H15B H 0.5927 0.2919 0.3806 0.107 Uiso 0.33 1 calc PR
H15C H 0.6992 0.4073 0.3806 0.107 Uiso 0.33 1 calc PR
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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
N5 Cu1 N2 109.71(12) . 3
N5 Cu1 N2 109.71(12) . 2
N2 Cu1 N2 109.23(13) 3 2
N5 Cu1 N2 109.71(12) . .
N2 Cu1 N2 109.23(13) 3 .
N2 Cu1 N2 109.23(13) 2 .
C11 Cu2 N1 118.3(3) . .
C11 Cu2 N4 114.5(3) . 3_665
N1 Cu2 N4 115.88(18) . 3_665
C11 Cu2 N3 120.6(3) . .
N1 Cu2 N3 79.44(17) . .
N4 Cu2 N3 102.75(17) 3_665 .
F6B P1 F4A 153.5(6) . .
F6B P1 F5B 91.8(8) . .
F4A P1 F5B 104.7(7) . .
F6B P1 F2A 91.9(7) . .
F4A P1 F2A 106.3(6) . .
F5B P1 F2A 96.4(8) . .
F6B P1 F1A 70.9(6) . .
F4A P1 F1A 90.7(5) . .
F5B P1 F1A 82.4(7) . .
F2A P1 F1A 162.6(6) . .
F6B P1 F5A 107.4(7) . .
F4A P1 F5A 91.2(6) . .
F5B P1 F5A 15.9(7) . .
F2A P1 F5A 92.6(6) . .
F1A P1 F5A 90.6(6) . .
F6B P1 F3B 97.4(8) . .
F4A P1 F3B 68.0(6) . .
F5B P1 F3B 170.2(8) . .
F2A P1 F3B 80.0(6) . .
F1A P1 F3B 103.8(6) . .
F5A P1 F3B 154.4(7) . .
F6B P1 F3A 66.6(7) . .
F4A P1 F3A 94.2(5) . .
F5B P1 F3A 158.1(7) . .
F2A P1 F3A 88.7(5) . .
F1A P1 F3A 86.5(5) . .
F5A P1 F3A 174.0(6) . .
F3B P1 F3A 31.6(5) . .
F6B P1 F1B 91.3(7) . .
F4A P1 F1B 68.6(6) . .
F5B P1 F1B 89.8(9) . .
F2A P1 F1B 172.9(7) . .
F1A P1 F1B 22.1(6) . .
F5A P1 F1B 92.5(7) . .
F3B P1 F1B 93.3(7) . .
F3A P1 F1B 86.8(6) . .
F6B P1 F4B 176.4(7) . .
F4A P1 F4B 25.2(5) . .
F5B P1 F4B 86.6(8) . .
F2A P1 F4B 91.5(7) . .
F1A P1 F4B 105.7(6) . .
F5A P1 F4B 71.2(7) . .
F3B P1 F4B 84.4(7) . .
F3A P1 F4B 114.7(7) . .
F1B P1 F4B 85.4(7) . .
F6B P1 F2B 111.2(9) . .
F4A P1 F2B 89.3(7) . .
F5B P1 F2B 91.4(8) . .
F2A P1 F2B 19.7(6) . .
F1A P1 F2B 173.6(6) . .
F5A P1 F2B 83.0(7) . .
F3B P1 F2B 82.1(7) . .
F3A P1 F2B 99.9(6) . .
F1B P1 F2B 157.4(9) . .
F4B P1 F2B 72.1(8) . .
F6B P1 F6A 27.2(5) . .
F4A P1 F6A 179.2(5) . .
F5B P1 F6A 75.1(7) . .
F2A P1 F6A 73.0(6) . .
F1A P1 F6A 90.1(5) . .
F5A P1 F6A 88.5(5) . .
F3B P1 F6A 112.2(6) . .
F3A P1 F6A 86.2(5) . .
F1B P1 F6A 112.1(6) . .
F4B P1 F6A 154.1(6) . .
F2B P1 F6A 90.0(7) . .
F7 P2 F7 89.5(3) . 3_565
F7 P2 F7 89.5(3) . 2_665
F7 P2 F7 89.5(3) 3_565 2_665
F7 P2 F8 90.5(3) . .
F7 P2 F8 91.0(3) 3_565 .
F7 P2 F8 179.5(4) 2_665 .
F7 P2 F8 91.0(3) . 2_665
F7 P2 F8 179.5(4) 3_565 2_665
F7 P2 F8 90.5(3) 2_665 2_665
F8 P2 F8 89.0(3) . 2_665
F7 P2 F8 179.5(4) . 3_565
F7 P2 F8 90.5(3) 3_565 3_565
F7 P2 F8 91.0(3) 2_665 3_565
F8 P2 F8 89.0(3) . 3_565
F8 P2 F8 89.0(3) 2_665 3_565
F1B F1A P1 82(2) . .
F2B F2A P1 87(2) . .
F3B F3A P1 73.2(11) . .
F3B F3A F6B 125.2(14) . .
P1 F3A F6B 53.8(6) . .
F4B F4A P1 84.7(17) . .
F4B F4A F3B 117.8(17) . .
P1 F4A F3B 57.6(6) . .
F6B F6A P1 66.6(15) . .
F1A F1B P1 76(2) . .
F2A F2B P1 73(2) . .
F3A F3B P1 75.2(12) . .
F3A F3B F4A 119.1(14) . .
P1 F3B F4A 54.5(5) . .
F4A F4B P1 70.1(16) . .
F6A F6B P1 86.1(15) . .
F6A F6B F3A 123.5(17) . .
P1 F6B F3A 59.6(6) . .
C4 N1 C1 116.4(5) . .
C4 N1 Cu2 115.3(3) . .
C1 N1 Cu2 128.3(3) . .
C1 N2 C2 117.7(5) . .
C1 N2 Cu1 117.2(4) . .
C2 N2 Cu1 124.2(4) . .
C6 N3 C9 116.1(5) . .
C6 N3 Cu2 130.1(4) . .
C9 N3 Cu2 113.8(4) . .
C6 N4 C7 117.2(5) . .
C6 N4 Cu2 117.6(4) . 2_655
C7 N4 Cu2 125.2(4) . 2_655
N2 C1 N1 125.4(5) . .
N2 C2 C3 120.5(5) . .
N2 C2 C5 119.0(5) . .
C3 C2 C5 120.5(5) . .
C4 C3 C2 118.6(5) . .
N1 C4 C3 121.2(5) . .
N1 C4 C9 115.8(5) . .
C3 C4 C9 122.9(5) . .
N3 C6 N4 127.1(5) . .
N4 C7 C8 119.2(5) . .
N4 C7 C10 119.9(5) . .
C8 C7 C10 120.8(5) . .
C9 C8 C7 118.9(5) . .
C8 C9 N3 121.2(5) . .
C8 C9 C4 123.2(5) . .
N3 C9 C4 115.6(5) . .
O1 C11 Cu2 179.8(9) . .
C12 N5 Cu1 180.000(2) . .
N5 C12 C13 180.000(3) . .
N6 C14 C15 180.000(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N5 1.946(10) .
Cu1 N2 2.060(4) 3
Cu1 N2 2.060(4) 2
Cu1 N2 2.060(4) .
Cu2 C11 1.822(8) .
Cu2 N1 2.066(5) .
Cu2 N4 2.070(5) 3_665
Cu2 N3 2.100(4) .
P1 F6B 1.518(15) .
P1 F4A 1.550(10) .
P1 F5B 1.56(2) .
P1 F2A 1.576(11) .
P1 F1A 1.593(10) .
P1 F5A 1.595(12) .
P1 F3B 1.607(14) .
P1 F3A 1.624(9) .
P1 F1B 1.627(15) .
P1 F4B 1.641(15) .
P1 F2B 1.648(15) .
P1 F6A 1.650(10) .
P2 F7 1.555(5) .
P2 F7 1.555(5) 3_565
P2 F7 1.555(5) 2_665
P2 F8 1.595(5) .
P2 F8 1.595(5) 2_665
P2 F8 1.595(5) 3_565
F1A F1B 0.619(17) .
F2A F2B 0.557(16) .
F3A F3B 0.881(15) .
F3A F6B 1.728(18) .
F4A F4B 0.702(14) .
F4A F3B 1.765(17) .
F6A F6B 0.757(13) .
N1 C4 1.356(7) .
N1 C1 1.363(7) .
N2 C1 1.338(7) .
N2 C2 1.352(7) .
N3 C6 1.314(7) .
N3 C9 1.367(7) .
N4 C6 1.334(7) .
N4 C7 1.350(7) .
N4 Cu2 2.070(5) 2_655
N6 C14 1.10(2) .
C2 C3 1.394(8) .
C2 C5 1.503(7) .
C3 C4 1.388(7) .
C4 C9 1.480(7) .
C7 C8 1.410(8) .
C7 C10 1.477(8) .
C8 C9 1.357(8) .
O1 C11 1.129(9) .
N5 C12 1.142(15) .
C12 C13 1.433(16) .
C14 C15 1.45(2) .
