#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180128 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/26/7102630.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_7102630
loop_
_publ_author_name
'Jaume Veciana'
'Daniel Maspoch'
'Concepcio Rovira'
'Daniel Ruiz-Molina'
'Klaus Wurst'
_publ_section_title
;
A new (63).(69.81) non-interpenetrated paramagnetic
network with helical nanochannels based on a tricarboxylic
perchlorotriphenylmethyl radical
;
_journal_issue                   10
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1164
_journal_page_last               1165
_journal_paper_doi               10.1039/b315147f
_journal_year                    2004
_chemical_formula_sum            'C44 H54 Cl12 Co N2 O17'
_chemical_formula_weight         1367.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.312(4)
_cell_length_b                   15.887(2)
_cell_length_c                   16.428(2)
_cell_measurement_reflns_used    10641
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      1.0
_cell_volume                     7650.2(17)
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.869
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       phi-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  0.1049
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10784
_diffrn_reflns_theta_full        19.00
_diffrn_reflns_theta_max         19.00
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2796
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.034(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.361
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         2687
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.360
_refine_ls_R_factor_all          0.1880
_refine_ls_R_factor_gt           0.1363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3477
_refine_ls_wR_factor_ref         0.3783
_reflns_number_gt                1635
_reflns_number_total             2687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b315147f.txt
_cod_data_source_block           mor
_cod_original_sg_symbol_H-M      Pnna
_cod_database_code               7102630
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-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
Co1 Co 0.49178(12) 0.2500 0.2500 0.1026(18) Uani 1 2 d S
N1 N 0.4925(6) 0.3459(9) 0.3484(8) 0.111(5) Uani 1 1 d .
O1 O 0.5622(8) 0.2500 0.2500 0.101(5) Uani 1 2 d S
O2 O 0.5795(12) 0.1584(18) 0.3519(19) 0.167(13) Uani 0.50 1 d P
O3 O 0.8758(8) 0.2654(16) -0.1092(12) 0.234(10) Uani 1 1 d .
O4 O 0.9243(10) 0.336(2) -0.0464(14) 0.251(13) Uani 1 1 d .
O5 O 0.4211(6) 0.2500 0.2500 0.122(6) Uani 1 2 d S
O6 O 0.4884(4) 0.1547(6) 0.3370(6) 0.114(4) Uani 1 1 d .
Cl1B Cl 0.6371(5) 0.1539(11) 0.1139(10) 0.166(6) Uani 0.50 1 d P
Cl1A Cl 0.6306(5) 0.0947(9) 0.1715(11) 0.161(5) Uani 0.50 1 d P
Cl2 Cl 0.7387(2) 0.1214(4) 0.1427(4) 0.180(3) Uani 1 1 d .
Cl3 Cl 0.8589(3) 0.1203(4) 0.2143(4) 0.183(3) Uani 1 1 d .
Cl4 Cl 0.9163(3) 0.1514(6) 0.0589(5) 0.222(4) Uani 1 1 d .
Cl5 Cl 0.8135(5) 0.4110(7) -0.0214(5) 0.321(7) Uani 1 1 d .
Cl6 Cl 0.7596(3) 0.3954(6) 0.1400(4) 0.233(5) Uani 1 1 d .
C1 C 0.5906(13) 0.206(2) 0.294(2) 0.088(9) Uani 0.50 1 d P
C2 C 0.6405(15) 0.220(2) 0.2808(17) 0.093(11) Uani 0.50 1 d P
C3A C 0.6600(16) 0.185(4) 0.214(4) 0.13(2) Uani 0.50 1 d P
C3B C 0.669(4) 0.223(3) 0.170(2) 0.14(3) Uani 0.50 1 d P
C4 C 0.7100(13) 0.1943(19) 0.2011(16) 0.170(12) Uani 1 1 d .
C5 C 0.7386(13) 0.2500 0.2500 0.121(9) Uani 1 2 d S
C6 C 0.7853(11) 0.2500 0.2500 0.121(9) Uani 1 2 d S
C7 C 0.8092(8) 0.2583(16) 0.1715(12) 0.140(8) Uani 1 1 d .
C8 C 0.8462(8) 0.2013(14) 0.1527(12) 0.132(7) Uani 1 1 d .
C9 C 0.8730(9) 0.2091(16) 0.0819(17) 0.148(9) Uani 1 1 d .
C10 C 0.8632(10) 0.273(3) 0.0286(17) 0.213(17) Uani 1 1 d .
C11 C 0.8264(13) 0.3282(18) 0.0424(13) 0.180(11) Uani 1 1 d .
C12 C 0.8027(8) 0.3234(16) 0.1142(17) 0.165(9) Uani 1 1 d .
C13 C 0.891(2) 0.299(2) -0.046(2) 0.23(2) Uani 1 1 d .
C14 C 0.4694(8) 0.4153(13) 0.3412(11) 0.142(9) Uani 1 1 d .
C15 C 0.4738(8) 0.4761(11) 0.4008(15) 0.134(7) Uani 1 1 d .
C16 C 0.4978(7) 0.4677(10) 0.4666(11) 0.089(5) Uani 1 1 d .
C17 C 0.5213(7) 0.3955(13) 0.4728(11) 0.118(6) Uani 1 1 d .
C18 C 0.5189(7) 0.3335(10) 0.4108(11) 0.115(6) Uani 1 1 d .
O7 O 0.578(4) 0.137(5) 0.469(6) 0.47(5) Uiso 0.50 1 d P
O8 O 0.619(3) 0.069(5) 0.342(5) 0.41(4) Uiso 0.50 1 d P
O9 O 0.956(2) 0.423(3) 0.095(4) 0.51(3) Uiso 1 1 d D
C19 C 0.966(3) 0.359(3) 0.147(4) 0.37(3) Uiso 1 1 d D
C20 C 0.993(5) 0.399(7) 0.211(6) 0.70(10) Uiso 1 1 d D
O10 O 0.610(3) 0.002(4) 0.704(5) 0.36(3) Uiso 0.50 1 d PD
C21 C 0.603(3) 0.017(7) 0.625(5) 0.33(4) Uiso 0.50 1 d PD
C22 C 0.640(7) 0.069(16) 0.596(10) 0.8(2) Uiso 0.50 1 d PD
O11 O 0.817(2) 0.107(3) -0.128(4) 0.53(3) Uiso 1 1 d D
C23 C 0.8103(19) 0.069(3) -0.049(3) 0.36(3) Uiso 1 1 d D
C24 C 0.837(2) -0.008(3) -0.059(3) 0.35(2) Uiso 1 1 d D
O12 O 0.275(3) 0.126(4) 0.250(4) 0.37(4) Uiso 0.50 1 d PD
C25 C 0.303(3) 0.192(7) 0.269(8) 0.38(6) Uiso 0.50 1 d PD
C26 C 0.273(5) 0.260(5) 0.294(7) 0.37(6) Uiso 0.50 1 d PD
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 '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
O5 Co1 O1 180.000(1) . .
O5 Co1 O6 87.3(3) . 4
O1 Co1 O6 92.7(3) . 4
O5 Co1 O6 87.3(3) . .
O1 Co1 O6 92.7(3) . .
O6 Co1 O6 174.6(7) 4 .
O5 Co1 N1 90.5(5) . 4
O1 Co1 N1 89.5(5) . 4
O6 Co1 N1 90.0(5) 4 4
O6 Co1 N1 90.1(5) . 4
O5 Co1 N1 90.5(5) . .
O1 Co1 N1 89.5(5) . .
O6 Co1 N1 90.1(5) 4 .
O6 Co1 N1 90.0(5) . .
N1 Co1 N1 178.9(9) 4 .
C14 N1 C18 120.7(15) . .
C14 N1 Co1 120.7(13) . .
C18 N1 Co1 118.4(13) . .
C1 O1 C1 101(4) 4 .
C1 O1 Co1 130(2) 4 .
C1 O1 Co1 130(2) . .
Cl1A Cl1B C3B 98.5(17) . .
Cl1A Cl1B C3A 67(2) . .
C3B Cl1B C3A 31.7(18) . .
Cl1B Cl1A C3A 70(3) . .
Cl1B Cl1A C3B 46.8(13) . .
C3A Cl1A C3B 23(3) . .
O2 C1 O1 125(4) . .
O2 C1 C2 117(3) . .
O1 C1 C2 117(4) . .
C2 C2 C3B 88(3) 4 4
C2 C2 C3A 72(4) 4 .
C3B C2 C3A 117(4) 4 .
C2 C2 C1 102(2) 4 .
C3B C2 C1 125(4) 4 .
C3A C2 C1 118(3) . .
C2 C2 C3A 53(3) 4 4
C3B C2 C3A 36(2) 4 4
C3A C2 C3A 106(3) . 4
C1 C2 C3A 118(3) . 4
C2 C2 C3B 47(2) 4 .
C3B C2 C3B 104(5) 4 .
C3A C2 C3B 26(4) . .
C1 C2 C3B 124(4) . .
C3A C2 C3B 83(3) 4 .
C3B C3A C2 117(8) . .
C3B C3A C4 64(6) . .
C2 C3A C4 119(4) . .
C3B C3A C2 63(7) . 4
C2 C3A C2 55(3) . 4
C4 C3A C2 105(4) . 4
C3B C3A Cl1A 110(7) . .
C2 C3A Cl1A 116(3) . .
C4 C3A Cl1A 120(3) . .
C2 C3A Cl1A 126(4) 4 .
C3B C3A Cl1B 68(7) . .
C2 C3A Cl1B 133(4) . .
C4 C3A Cl1B 105(3) . .
C2 C3A Cl1B 100(5) 4 .
Cl1A C3A Cl1B 43.4(11) . .
C3A C3B C2 80(6) . 4
C3A C3B C4 76(6) . .
C2 C3B C4 120(4) 4 .
C3A C3B Cl1B 81(7) . .
C2 C3B Cl1B 112(6) 4 .
C4 C3B Cl1B 117(4) . .
C3A C3B C2 37(4) . .
C2 C3B C2 44(2) 4 .
C4 C3B C2 91(3) . .
Cl1B C3B C2 104(4) . .
C3A C3B Cl1A 46(5) . .
C2 C3B Cl1A 105(5) 4 .
C4 C3B Cl1A 97(3) . .
Cl1B C3B Cl1A 34.8(15) . .
C2 C3B Cl1A 76(3) . .
C5 C4 C3A 123(3) . .
C5 C4 C3B 120(3) . .
C3A C4 C3B 40(3) . .
C5 C4 Cl2 116(3) . .
C3A C4 Cl2 119(2) . .
C3B C4 Cl2 116(3) . .
C6 C5 C4 125.0(18) . .
C6 C5 C4 125.0(18) . 4
C4 C5 C4 110(4) . 4
C5 C6 C7 118.3(16) . .
C5 C6 C7 118.3(16) . 4
C7 C6 C7 123(3) . 4
C12 C7 C8 114.7(18) . .
C12 C7 C6 126(2) . .
C8 C7 C6 119(2) . .
C9 C8 C7 122.7(18) . .
C9 C8 Cl3 116.1(19) . .
C7 C8 Cl3 121.2(17) . .
C10 C9 C8 118(2) . .
C10 C9 Cl4 116(2) . .
C8 C9 Cl4 126(2) . .
C9 C10 C11 121(2) . .
C9 C10 C13 127(4) . .
C11 C10 C13 112(4) . .
C12 C11 C10 119(2) . .
C12 C11 Cl5 117(3) . .
C10 C11 Cl5 123(3) . .
C11 C12 C7 123(2) . .
C11 C12 Cl6 122(2) . .
C7 C12 Cl6 114.5(19) . .
O4 C13 O3 122(3) . .
O4 C13 C10 127(4) . .
O3 C13 C10 111(4) . .
N1 C14 C15 118.8(18) . .
C16 C15 C14 124.6(18) . .
C15 C16 C17 115.5(16) . .
C15 C16 C16 126(2) . 5_666
C17 C16 C16 119(3) . 5_666
C16 C17 C18 120.9(17) . .
N1 C18 C17 119.3(16) . .
O9 C19 C20 104(3) . .
O10 C21 C22 108(3) . .
O11 C23 C24 101(3) . .
O12 C25 C26 84(8) . 4
O12 C25 C26 107(3) . .
C26 C25 C26 59(9) 4 .
O12 C25 C25 132(10) . 4
C26 C25 C25 48(6) 4 4
C26 C25 C25 52(7) . 4
C26 C26 C25 57(6) 4 4
C26 C26 C25 64(6) 4 .
C25 C26 C25 81(10) 4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O5 2.072(17) .
Co1 O1 2.06(2) .
Co1 O6 2.084(10) 4
Co1 O6 2.084(10) .
Co1 N1 2.222(13) 4
Co1 N1 2.222(13) .
N1 C14 1.30(2) .
N1 C18 1.30(2) .
O1 C1 1.31(4) 4
O1 C1 1.31(4) .
O2 C1 1.25(4) .
O3 C13 1.25(4) .
O4 C13 1.13(4) .
Cl1B Cl1A 1.348(18) .
Cl1B C3B 1.72(8) .
Cl1B C3A 1.84(6) .
Cl1A C3A 1.81(4) .
Cl1A C3B 2.34(8) .
Cl2 C4 1.72(2) .
Cl3 C8 1.68(2) .
Cl4 C9 1.61(2) .
Cl5 C11 1.72(3) .
Cl6 C12 1.75(2) .
C1 C2 1.49(5) .
C2 C2 1.40(6) 4
C2 C3B 1.47(7) 4
C2 C3A 1.36(5) .
C2 C3A 1.62(8) 4
C2 C3B 2.00(6) .
C3A C3B 0.98(6) .
C3A C4 1.49(5) .
C3A C2 1.62(8) 4
C3B C2 1.47(7) 4
C3B C4 1.38(9) .
C4 C5 1.46(4) .
C5 C6 1.37(4) .
C5 C4 1.46(4) 4
C6 C7 1.47(3) .
C6 C7 1.47(3) 4
C7 C12 1.41(3) .
C7 C8 1.45(3) .
C8 C9 1.41(3) .
C9 C10 1.37(4) .
C10 C11 1.41(4) .
C10 C13 1.54(5) .
C11 C12 1.37(3) .
C14 C15 1.38(2) .
C15 C16 1.30(2) .
C16 C17 1.34(2) .
C16 C16 1.51(3) 5_666
C17 C18 1.42(2) .
O9 C19 1.37(3) .
C19 C20 1.47(3) .
O10 C21 1.35(3) .
C21 C22 1.45(3) .
O11 C23 1.44(3) .
C23 C24 1.45(3) .
O12 C25 1.35(3) .
C25 C26 1.55(12) 4
C25 C26 1.45(3) .
C25 C25 1.9(2) 4
C26 C26 1.5(2) 4
C26 C25 1.55(12) 4
