#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:32:27 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180477 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/46/7214647.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_7214647
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            'C48 H56 B4 Cu4 F16 N16 O8'
_chemical_formula_weight         1586.49
_chemical_name_systematic
;
?
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-12-14T21:22:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9479(9)
_cell_length_b                   12.9479(9)
_cell_length_c                   40.274(3)
_cell_measurement_reflns_used    9091
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.2771
_cell_measurement_theta_min      2.2243
_cell_volume                     6751.9(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            20146
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.08
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         4141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0764P)²+5.4638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                3900
_reflns_number_total             4141
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2ce25211b.txt
_cod_data_source_block           '[Cu4(Me2bpm)4(CO)4](BF4)4_4MeOH'
_cod_database_code               7214647
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, -z+1/4'
'-x, -y, z'
'-x, y+1/2, -z+1/4'
'-y+1/2, -x, z+3/4'
'-y, x, -z'
'y, -x, -z'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1, -z+3/4'
'-y+1, -x+1/2, z+5/4'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'y+1, x+1/2, z+5/4'
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 0.21020(3) 0.30978(3) 0.213649(8) 0.02415(12) Uani 1 1 d .
F1 F 0.0295(3) 0.5832(3) 0.19285(8) 0.0774(11) Uani 1 1 d .
F2 F 0.0823(2) 0.4705(2) 0.15369(6) 0.0500(6) Uani 1 1 d .
B1 B 0 0.5 0.17326(14) 0.0376(13) Uani 1 2 d S
F3A F 0.4800(5) 0.2554(4) 0.15984(14) 0.0582(8) Uani 0.514(4) 1 d P
F4A F 0.5907(5) 0.3129(5) 0.12211(13) 0.0582(8) Uani 0.514(4) 1 d P
F3B F 0.5387(5) 0.3538(5) 0.12677(15) 0.0582(8) Uani 0.486(4) 1 d P
F4B F 0.4255(5) 0.2305(5) 0.14222(14) 0.0582(8) Uani 0.486(4) 1 d P
B2 B 0.5082(6) 0.25 0.125 0.0389(13) Uani 1 2 d S
O1 O 0.1317(3) 0.1972(3) 0.15612(8) 0.0646(8) Uani 1 1 d .
O2 O 0.4004(8) 0.4617(8) 0.2824(2) 0.081(3) Uani 0.5 1 d P
H2 H 0.3916 0.4794 0.3018 0.122 Uiso 0.5 1 calc PR
O3 O 0.4071(10) 0.3853(7) 0.3466(2) 0.093(4) Uani 0.5 1 d P
H3 H 0.4354 0.4386 0.3528 0.14 Uiso 0.5 1 calc PR
N1 N 0.1217(2) 0.2817(2) 0.25572(6) 0.0229(5) Uani 1 1 d .
N2 N 0.3223(2) 0.2522(2) 0.24510(6) 0.0227(5) Uani 1 1 d .
N3 N 0.4922(2) 0.2065(3) 0.26138(7) 0.0375(7) Uani 1 1 d .
N4 N -0.0351(2) 0.2596(2) 0.28550(6) 0.0258(5) Uani 1 1 d .
C1 C 0.4236(3) 0.2419(3) 0.24013(8) 0.0286(7) Uani 1 1 d .
H1 H 0.4485 0.2618 0.2194 0.034 Uiso 1 1 calc R
C2 C 0.4567(3) 0.1772(3) 0.29118(8) 0.0357(8) Uani 1 1 d .
C3 C 0.5341(3) 0.1359(6) 0.31598(12) 0.0723(19) Uani 1 1 d .
H3A H 0.5729 0.0808 0.306 0.108 Uiso 1 1 calc R
H3B H 0.4984 0.1105 0.3352 0.108 Uiso 1 1 calc R
H3C H 0.5803 0.1903 0.3224 0.108 Uiso 1 1 calc R
C4 C 0.3532(2) 0.1836(3) 0.29909(8) 0.0289(7) Uani 1 1 d .
H4 H 0.3289 0.163 0.3198 0.035 Uiso 1 1 calc R
C5 C 0.2868(2) 0.2219(2) 0.27496(7) 0.0214(5) Uani 1 1 d .
C6 C 0.1727(2) 0.2327(2) 0.28030(7) 0.0220(6) Uani 1 1 d .
C7 C 0.1226(2) 0.1955(3) 0.30782(7) 0.0283(6) Uani 1 1 d .
H7 H 0.1586 0.1617 0.3246 0.034 Uiso 1 1 calc R
C8 C 0.0156(2) 0.2098(3) 0.30997(7) 0.0269(6) Uani 1 1 d .
C9 C 0.0202(2) 0.2926(3) 0.25949(7) 0.0263(6) Uani 1 1 d .
H9 H -0.0155 0.3261 0.2426 0.032 Uiso 1 1 calc R
C10 C -0.0445(3) 0.1718(3) 0.33912(9) 0.0386(9) Uani 1 1 d .
H10A H -0.0788 0.2289 0.3496 0.058 Uiso 1 1 calc R
H10B H 0.0015 0.1397 0.3547 0.058 Uiso 1 1 calc R
H10C H -0.0949 0.1224 0.3318 0.058 Uiso 1 1 calc R
C11 C 0.1632(5) 0.2414(4) 0.17688(12) 0.0646(8) Uani 1 1 d .
C12 C 0.5 0.5 0.2708(4) 0.113(4) Uani 1 2 d S
C13 C 0.3007(15) 0.3795(11) 0.3613(3) 0.090(4) Uani 0.5 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
B B 0.0013 0.0007 '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'
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
C11 Cu1 N4 123.50(19) . 14
C11 Cu1 N2 123.8(2) . .
N4 Cu1 N2 102.09(11) 14 .
C11 Cu1 N1 113.1(2) . .
N4 Cu1 N1 105.29(10) 14 .
N2 Cu1 N1 79.90(10) . .
F2 B1 F2 110.3(4) 3_565 .
F2 B1 F1 108.84(19) 3_565 .
F2 B1 F1 109.0(2) . .
F2 B1 F1 109.0(2) 3_565 3_565
F2 B1 F1 108.84(19) . 3_565
F1 B1 F1 110.8(5) . 3_565
B2 F4A F4A 52.4(4) . 2
B2 F4B F4B 55.4(4) . 2
F4B B2 F4B 69.2(7) 2 .
F4B B2 F4A 119.3(4) 2 .
F4B B2 F4A 144.6(3) . .
F4B B2 F4A 144.6(3) 2 2
F4B B2 F4A 119.3(4) . 2
F4A B2 F4A 75.2(7) . 2
F4B B2 F3B 113.0(4) 2 2
F4B B2 F3B 94.2(4) . 2
F4A B2 F3B 110.6(7) . 2
F4A B2 F3B 37.1(3) 2 2
F4B B2 F3B 94.2(4) 2 .
F4B B2 F3B 113.0(4) . .
F4A B2 F3B 37.1(3) . .
F4A B2 F3B 110.6(7) 2 .
F3B B2 F3B 147.3(8) 2 .
F4B B2 F3A 44.5(4) 2 2
F4B B2 F3A 107.5(6) . 2
F4A B2 F3A 98.3(4) . 2
F4A B2 F3A 104.7(4) 2 2
F3B B2 F3A 88.6(3) 2 2
F3B B2 F3A 99.5(4) . 2
F4B B2 F3A 107.5(6) 2 .
F4B B2 F3A 44.5(4) . .
F4A B2 F3A 104.7(4) . .
F4A B2 F3A 98.3(4) 2 .
F3B B2 F3A 99.5(4) 2 .
F3B B2 F3A 88.6(3) . .
F3A B2 F3A 150.9(8) 2 .
C12 O2 H2 109.5 . .
C13 O3 H3 109.5 . .
C9 N1 C6 116.8(2) . .
C9 N1 Cu1 128.28(19) . .
C6 N1 Cu1 114.2(2) . .
C1 N2 C5 116.1(3) . .
C1 N2 Cu1 129.5(2) . .
C5 N2 Cu1 114.4(2) . .
C1 N3 C2 116.7(3) . .
C9 N4 C8 117.6(3) . .
C9 N4 Cu1 118.5(2) . 15_455
C8 N4 Cu1 123.9(2) . 15_455
N3 C1 N2 127.0(3) . .
N3 C1 H1 116.5 . .
N2 C1 H1 116.5 . .
N3 C2 C4 121.6(3) . .
N3 C2 C3 117.6(3) . .
C4 C2 C3 120.8(3) . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 C5 117.5(3) . .
C2 C4 H4 121.3 . .
C5 C4 H4 121.3 . .
N2 C5 C4 121.2(3) . .
N2 C5 C6 115.9(3) . .
C4 C5 C6 122.9(3) . .
N1 C6 C7 121.7(3) . .
N1 C6 C5 114.9(3) . .
C7 C6 C5 123.3(3) . .
C6 C7 C8 118.1(3) . .
C6 C7 H7 120.9 . .
C8 C7 H7 120.9 . .
N4 C8 C7 120.0(3) . .
N4 C8 C10 118.6(3) . .
C7 C8 C10 121.4(3) . .
N1 C9 N4 125.7(3) . .
N1 C9 H9 117.1 . .
N4 C9 H9 117.1 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O1 C11 Cu1 175.8(6) . .
O2 C12 O2 142.5(15) . 3_665
O3 C13 C13 162.8(15) . 12_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 C11 1.830(5) .
Cu1 N4 2.046(3) 14
Cu1 N2 2.065(3) .
Cu1 N1 2.078(2) .
F1 B1 1.389(4) .
F2 B1 1.379(4) .
B1 F2 1.379(4) 3_565
B1 F1 1.389(4) 3_565
F3A B2 1.451(5) .
F4A B2 1.349(8) .
F4A F4A 1.646(12) 2
F3B B2 1.403(6) .
F4B B2 1.300(8) .
F4B F4B 1.476(12) 2
B2 F4B 1.300(8) 2
B2 F4A 1.349(8) 2
B2 F3B 1.403(6) 2
B2 F3A 1.451(5) 2
O1 C11 1.092(6) .
O2 C12 1.460(12) .
O2 H2 0.82 .
O3 C13 1.50(2) .
O3 H3 0.82 .
N1 C9 1.330(4) .
N1 C6 1.349(4) .
N2 C1 1.334(4) .
N2 C5 1.346(4) .
N3 C1 1.316(5) .
N3 C2 1.340(4) .
N4 C9 1.339(4) .
N4 C8 1.349(4) .
N4 Cu1 2.046(3) 15_455
C1 H1 0.93 .
C2 C4 1.379(5) .
C2 C3 1.513(5) .
C3 H3A 0.96 .
C3 H3B 0.96 .
C3 H3C 0.96 .
C4 C5 1.389(4) .
C4 H4 0.93 .
C5 C6 1.499(4) .
C6 C7 1.372(4) .
C7 C8 1.400(4) .
C7 H7 0.93 .
C8 C10 1.492(4) .
C9 H9 0.93 .
C10 H10A 0.96 .
C10 H10B 0.96 .
C10 H10C 0.96 .
C12 O2 1.460(12) 3_665
C13 C13 1.72(4) 12_545
