#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/46/7114678.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_7114678
loop_
_publ_author_name
'Carlucci, Lucia'
'Ciani, Gianfranco'
'Proserpio, Davide M.'
'Rizzato, Silvia'
_publ_section_title
;
 Interlinked molecular squares with [Cu(2,2′-bipy)]2+ corners
 generating a three-dimensional network of unprecedented topological type
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1198
_journal_paper_doi               10.1039/b103736f
_journal_year                    2001
_chemical_formula_sum            'C44 H57 B3 Cl Cu2 F12 N8 O8.5'
_chemical_formula_weight         1256.94
_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
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   21.479(2)
_cell_length_b                   21.479(2)
_cell_length_c                   29.303(3)
_cell_measurement_reflns_used    917
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.
_cell_measurement_theta_min      2.
_cell_volume                     13519(2)
_computing_molecular_graphics    SCHAKAL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      223(2)
_diffrn_detector_type            CCD_plate
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       SMART
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25456
_diffrn_reflns_theta_full        24.03
_diffrn_reflns_theta_max         24.
_diffrn_reflns_theta_min         2.
_diffrn_standards_decay_%        2
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube-like
_exptl_crystal_F_000             5144
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.175
_refine_diff_density_min         -0.457
_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   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5073
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1790
_refine_ls_R_factor_obs          0.0982
_refine_ls_shift/su_max          0.641
_refine_ls_shift/su_mean         0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1617P)²+82.2720P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3268
_refine_ls_wR_factor_obs         0.2450
_reflns_number_observed          2933
_reflns_number_total             5073
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b103736f.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      I-42d
_cod_original_formula_sum        'C44 H57 B3 Cl Cu2 F12 N8 O8.50'
_cod_database_code               7114678
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_nazim  4.94
_diffrn_measurement_domega       0.30
_diffrn_measurement_rtime        54
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y+1/2, -z+1/4'
'-x, y+1/2, -z+1/4'
'y, x+1/2, z+1/4'
'-y, -x+1/2, z+1/4'
'-y, x, -z'
'y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, y+1, -z+3/4'
'y+1/2, x+1, z+3/4'
'-y+1/2, -x+1, z+3/4'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
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
O1S O 0.0539(10) 0.4798(10) 0.7986(7) 0.188(6) Uiso 1 1 d .
O2S O -0.0311(17) 0.268(2) 0.6096(12) 0.188(6) Uiso 0.50 1 d P
O3S O 0.102(2) 0.5660(19) 0.7492(14) 0.188(6) Uiso 0.50 1 d P
O4S O 0.149(4) 0.574(4) 0.708(3) 0.188(6) Uiso 0.25 1 d P
O5S O 0.025(3) 0.506(5) 0.901(2) 0.188(6) Uiso 0.25 1 d P
O6S O 0.345(4) 0.900(4) 0.133(3) 0.188(6) Uiso 0.25 1 d P
O7S O -0.030(4) 0.328(4) 0.600(3) 0.188(6) Uiso 0.25 1 d P
O8S O 0.452(4) 0.282(3) 0.119(3) 0.188(6) Uiso 0.25 1 d P
C12 C 0.1860(9) 0.0237(8) 0.8013(7) 0.106(6) Uani 1 1 d .
H12 H 0.1476 0.0435 0.7991 0.128 Uiso 1 1 calc R
C13 C 0.1897(17) -0.0421(11) 0.8106(9) 0.151(11) Uani 1 1 d .
H13 H 0.1534 -0.0657 0.8109 0.181 Uiso 1 1 calc R
C14 C 0.2410(17) -0.0682(10) 0.8184(9) 0.141(10) Uani 1 1 d .
H14 H 0.2420 -0.1103 0.8257 0.169 Uiso 1 1 calc R
C15 C 0.2986(13) -0.0333(9) 0.8163(8) 0.132(8) Uani 1 1 d .
H15 H 0.3372 -0.0513 0.8218 0.159 Uiso 1 1 calc R
C16 C 0.2919(8) 0.0268(7) 0.8056(6) 0.087(5) Uani 1 1 d .
C17 C 0.3483(8) 0.0704(8) 0.8053(6) 0.098(5) Uani 1 1 d .
C18 C 0.4087(10) 0.0535(13) 0.8147(11) 0.165(11) Uani 1 1 d .
H18 H 0.4183 0.0118 0.8196 0.198 Uiso 1 1 calc R
C19 C 0.4553(11) 0.0979(16) 0.8168(9) 0.151(10) Uani 1 1 d .
H19 H 0.4940 0.0885 0.8294 0.181 Uiso 1 1 calc R
N21 N 0.1538(5) 0.1599(5) 0.7793(5) 0.071(3) Uani 1 1 d D
C22 C 0.1165(7) 0.1681(8) 0.8128(9) 0.129(8) Uani 1 1 d D
H22 H 0.1331 0.1702 0.8421 0.154 Uiso 1 1 calc R
C23 C 0.0523(10) 0.1740(10) 0.8078(10) 0.155(11) Uani 1 1 d D
H23 H 0.0282 0.1801 0.8338 0.186 Uiso 1 1 calc R
C24 C 0.0233(7) 0.1713(13) 0.7666(10) 0.147(10) Uani 1 1 d D
C25 C 0.0657(10) 0.1643(13) 0.7291(10) 0.160(10) Uani 1 1 d D
H25 H 0.0508 0.1655 0.6994 0.192 Uiso 1 1 calc R
C26 C 0.1303(7) 0.1555(10) 0.7371(8) 0.118(7) Uani 1 1 d D
H26 H 0.1566 0.1466 0.7127 0.142 Uiso 1 1 calc R
C27 C -0.0478(8) 0.1708(7) 0.7613(8) 0.134(8) Uani 1 1 d D
H27A H -0.0594 0.1571 0.7310 0.160 Uiso 1 1 calc R
H27B H -0.0665 0.1431 0.7836 0.160 Uiso 1 1 calc R
N31 N 0.2586(5) 0.2397(5) 0.7703(5) 0.078(3) Uani 1 1 d D
C32 C 0.2669(6) 0.2563(7) 0.7274(6) 0.084(4) Uani 1 1 d D
H32 H 0.2702 0.2251 0.7054 0.101 Uiso 1 1 calc R
C33 C 0.2710(7) 0.3166(7) 0.7134(7) 0.097(5) Uani 1 1 d D
H33 H 0.2793 0.3263 0.6831 0.117 Uiso 1 1 calc R
C34 C 0.2625(13) 0.3629(7) 0.7452(7) 0.130(9) Uani 1 1 d D
C35 C 0.2598(19) 0.3453(9) 0.7888(7) 0.219(18) Uani 1 1 d D
H35 H 0.2599 0.3751 0.8119 0.263 Uiso 1 1 calc R
C36 C 0.2570(16) 0.2815(8) 0.7999(7) 0.188(14) Uani 1 1 d D
H36 H 0.2538 0.2701 0.8304 0.225 Uiso 1 1 calc R
C37 C 0.2624(8) 0.4309(8) 0.7307(8) 0.148(9) Uani 1 1 d D
H37A H 0.2335 0.4549 0.7490 0.177 Uiso 1 1 calc R
H37B H 0.2510 0.4350 0.6988 0.177 Uiso 1 1 calc R
C110 C 0.4434(9) 0.1544(15) 0.8004(8) 0.139(9) Uani 1 1 d .
H110 H 0.4746 0.1838 0.7959 0.166 Uiso 1 1 calc R
C111 C 0.3839(6) 0.1663(9) 0.7909(6) 0.101(6) Uani 1 1 d .
H111 H 0.3748 0.2073 0.7832 0.121 Uiso 1 1 calc R
N11 N 0.2389(5) 0.0558(4) 0.7960(4) 0.077(3) Uani 1 1 d .
N112 N 0.3373(4) 0.1283(6) 0.7910(4) 0.074(3) Uani 1 1 d .
B1 B 0.3059(7) 0.1082(6) 0.6644(5) 0.121(9) Uani 1 1 d D
B2 B 0.5000 0.0000 0.5673(9) 0.19(3) Uani 1 2 d SD
F11 F 0.2619(5) 0.1093(5) 0.6975(4) 0.128(4) Uani 1 1 d D
F12 F 0.3611(6) 0.0952(6) 0.6856(5) 0.182(6) Uani 1 1 d D
F13 F 0.3113(7) 0.1643(5) 0.6442(4) 0.177(6) Uani 1 1 d D
F14 F 0.2916(6) 0.0649(5) 0.6330(4) 0.155(5) Uani 1 1 d D
F21 F 0.5410(6) -0.0309(8) 0.5941(7) 0.237(9) Uani 1 1 d D
F22 F 0.4693(8) -0.0409(6) 0.5408(7) 0.309(16) Uani 1 1 d D
Cl Cl 0.2500 0.16475(18) 0.8750 0.0684(11) Uani 1 2 d S
Cu Cu 0.24658(7) 0.14836(7) 0.78773(5) 0.0641(5) Uani 1 1 d .
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 0.0000 0.0000 '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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
O2S O2S O7S 143(7) 3_556 .
N11 C12 C13 119(2) . .
C14 C13 C12 121(3) . .
C13 C14 C15 121(2) . .
C16 C15 C14 115(2) . .
C15 C16 N11 126.6(19) . .
C15 C16 C17 120.4(19) . .
N11 C16 C17 113.0(12) . .
N112 C17 C18 118(2) . .
N112 C17 C16 115.6(14) . .
C18 C17 C16 125.8(18) . .
C19 C18 C17 121(2) . .
C110 C19 C18 118(2) . .
C22 N21 C26 118.8(14) . .
C22 N21 Cu 122.7(12) . .
C26 N21 Cu 118.4(11) . .
N21 C22 C23 124(2) . .
C22 C23 C24 123(2) . .
C23 C24 C25 113.1(17) . .
C23 C24 C27 123(2) . .
C25 C24 C27 124(2) . .
C26 C25 C24 121(2) . .
N21 C26 C25 121(2) . .
C37 C27 C24 106.1(15) 16_456 .
C36 N31 C32 118.1(14) . .
C36 N31 Cu 120.9(12) . .
C32 N31 Cu 121.0(10) . .
N31 C32 C33 123.5(15) . .
C32 C33 C34 118.5(16) . .
C35 C34 C33 116.7(15) . .
C35 C34 C37 122.6(19) . .
C33 C34 C37 120.4(18) . .
C34 C35 C36 119.8(17) . .
N31 C36 C35 122.6(19) . .
C34 C37 C27 104.1(15) . 15_556
C111 C110 C19 116(2) . .
N112 C111 C110 128(2) . .
C12 N11 C16 117.4(13) . .
C12 N11 Cu 126.4(12) . .
C16 N11 Cu 114.8(10) . .
C111 N112 C17 116.9(14) . .
C111 N112 Cu 128.4(11) . .
C17 N112 Cu 112.8(10) . .
F14 B1 F13 109.7(11) . .
F14 B1 F11 110.1(11) . .
F13 B1 F11 111.1(10) . .
F14 B1 F12 111.5(11) . .
F13 B1 F12 107.9(11) . .
F11 B1 F12 106.5(11) . .
F22 B2 F22 109.5(15) . 2_655
F22 B2 F21 109.5(6) . .
F22 B2 F21 109.6(6) 2_655 .
F22 B2 F21 109.6(6) . 2_655
F22 B2 F21 109.5(6) 2_655 2_655
F21 B2 F21 109.1(15) . 2_655
B1 F11 Cu 139.9(8) . .
Cu Cl Cu 164.33(18) . 12_546
N112 Cu N11 82.0(5) . .
N112 Cu N21 173.2(5) . .
N11 Cu N21 93.1(5) . .
N112 Cu N31 95.5(5) . .
N11 Cu N31 172.0(5) . .
N21 Cu N31 88.7(5) . .
N112 Cu Cl 87.4(4) . .
N11 Cu Cl 91.0(4) . .
N21 Cu Cl 97.6(4) . .
N31 Cu Cl 96.5(4) . .
N112 Cu F11 82.3(4) . .
N11 Cu F11 80.0(4) . .
N21 Cu F11 92.1(5) . .
N31 Cu F11 92.1(4) . .
Cl Cu F11 167.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O2S O2S 1.18(7) 3_556
O2S O7S 1.32(9) .
O3S O4S 1.60(8) .
O5S O5S 1.10(15) 2_565
O8S O8S 1.42(13) 3
C12 N11 1.338(19) .
C12 C13 1.44(3) .
C13 C14 1.26(4) .
C14 C15 1.45(3) .
C15 C16 1.34(2) .
C16 N11 1.328(19) .
C16 C17 1.53(2) .
C17 N112 1.336(19) .
C17 C18 1.37(2) .
C18 C19 1.39(3) .
C19 C110 1.33(3) .
N21 C22 1.28(2) .
N21 C26 1.34(2) .
N21 Cu 2.023(11) .
C22 C23 1.39(3) .
C23 C24 1.36(3) .
C24 C25 1.44(3) .
C24 C27 1.533(10) .
C25 C26 1.42(2) .
C27 C37 1.524(10) 16_456
N31 C36 1.25(2) .
N31 C32 1.321(17) .
N31 Cu 2.043(11) .
C32 C33 1.36(2) .
C33 C34 1.37(2) .
C34 C35 1.33(2) .
C34 C37 1.522(10) .
C35 C36 1.41(3) .
C37 C27 1.524(10) 15_556
C110 C111 1.33(2) .
C111 N112 1.290(18) .
N11 Cu 2.009(10) .
N112 Cu 1.998(10) .
B1 F14 1.342(12) .
B1 F13 1.348(13) .
B1 F11 1.355(13) .
B1 F12 1.369(13) .
B2 F22 1.344(12) .
B2 F22 1.344(12) 2_655
B2 F21 1.354(12) .
B2 F21 1.354(12) 2_655
F11 Cu 2.794(10) .
Cl Cu 2.5825(17) .
Cl Cu 2.5825(17) 12_546
