#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:34:00 +0100 (vie 25 de mar de 2016) $
#$Revision: 179796 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/92/7009229.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_7009229
loop_
_publ_author_name
'Gleiter, Rolf'
'von Hirschheydt, Thomas'
'Wolfart, Volker'
'Rominger, Frank'
_publ_section_title
;
 Reaction of N,N'-bridged 1,10-diazacyclooctadeca-5,14-diynes with
 [CpCo(cod)]: a new type of superphane
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              685
_journal_paper_doi               10.1039/a909482b
_journal_year                    2000
_chemical_formula_sum            'C58 H90 Co2 N4'
_chemical_formula_weight         961.20
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.2140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.9708(16)
_cell_length_b                   9.4887(7)
_cell_length_c                   23.9264(17)
_cell_measurement_temperature    293(2)
_cell_volume                     5386.3(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19435
_diffrn_reflns_theta_full        25.59
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lamina
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .03
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4623
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1483
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.208
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0821P)²+12.7767P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.2032
_reflns_number_gt                2413
_reflns_number_total             4623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909482b.txt
_cod_data_source_block           4d
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009229
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.07327(3) 0.95940(9) -0.10556(3) 0.0694(3) Uani 1 1 d . . .
C1 C 0.0414(3) 1.1560(8) -0.1249(5) 0.105(2) Uani 1 1 d . . .
H1 H 0.0626 1.2385 -0.1233 0.126 Uiso 1 1 calc R . .
C2 C 0.0157(4) 1.0986(11) -0.0805(3) 0.108(3) Uani 1 1 d . . .
H2 H 0.0168 1.1352 -0.0443 0.130 Uiso 1 1 calc R . .
C3 C -0.0114(3) 0.9768(10) -0.1017(4) 0.108(3) Uani 1 1 d . . .
H3 H -0.0320 0.9170 -0.0816 0.130 Uiso 1 1 calc R . .
C4 C -0.0032(3) 0.9575(9) -0.1569(4) 0.102(2) Uani 1 1 d . . .
H4 H -0.0172 0.8836 -0.1803 0.122 Uiso 1 1 calc R . .
C5 C 0.0297(3) 1.0683(10) -0.1713(3) 0.096(2) Uani 1 1 d . . .
H5 H 0.0417 1.0814 -0.2062 0.116 Uiso 1 1 calc R . .
C6 C 0.1563(2) 0.9529(7) -0.0939(2) 0.0730(17) Uani 1 1 d . A .
C7 C 0.1315(2) 0.8310(7) -0.1244(2) 0.0755(17) Uani 1 1 d . . .
C8 C 0.1337(2) 0.7707(7) -0.1825(2) 0.0888(19) Uani 1 1 d . . .
H8A H 0.1154 0.8360 -0.2105 0.107 Uiso 1 1 calc R . .
H8B H 0.1125 0.6833 -0.1862 0.107 Uiso 1 1 calc R . .
C9 C 0.1934(2) 0.7418(7) -0.1950(2) 0.0808(18) Uani 1 1 d . . .
H9A H 0.1913 0.7109 -0.2339 0.097 Uiso 1 1 calc R . .
H9B H 0.2146 0.8293 -0.1913 0.097 Uiso 1 1 calc R . .
C10 C 0.2251(2) 0.6322(7) -0.1571(2) 0.0745(16) Uani 1 1 d . . .
H10A H 0.2190 0.6498 -0.1185 0.089 Uiso 1 1 calc R . .
H10B H 0.2098 0.5399 -0.1678 0.089 Uiso 1 1 calc R . .
N11 N 0.28522(18) 0.6305(5) -0.15922(17) 0.0677(13) Uani 1 1 d . A .
C12 C 0.3160(2) 0.5455(7) -0.1146(2) 0.0792(17) Uani 1 1 d . . .
H12A H 0.3535 0.5276 -0.1236 0.095 Uiso 1 1 calc R . .
H12B H 0.2971 0.4554 -0.1132 0.095 Uiso 1 1 calc R . .
C13 C 0.3209(2) 0.6151(7) -0.0565(2) 0.0776(17) Uani 1 1 d . . .
H13A H 0.3322 0.7127 -0.0593 0.093 Uiso 1 1 calc R . .
H13B H 0.2845 0.6137 -0.0433 0.093 Uiso 1 1 calc R . .
C14 C 0.1368(3) 0.9602(8) 0.0150(2) 0.092(2) Uani 1 1 d . . .
H14A H 0.1465 1.0595 0.0153 0.111 Uiso 1 1 calc R . .
H14B H 0.1000 0.9519 0.0271 0.111 Uiso 1 1 calc R . .
C15 C 0.1331(2) 0.9060(8) -0.0444(2) 0.0793(19) Uani 1 1 d . . .
C16 C 0.1090(2) 0.7847(8) -0.0748(3) 0.0810(18) Uani 1 1 d . . .
C17 C 0.0792(4) 0.6573(10) -0.0589(4) 0.148(4) Uani 1 1 d . . .
H17A H 0.0644 0.6815 -0.0244 0.177 Uiso 1 1 calc R . .
H17B H 0.0467 0.6461 -0.0878 0.177 Uiso 1 1 calc R . .
C19 C 0.3567(5) 1.0186(14) 0.0187(5) 0.235(8) Uani 1 1 d . A .
H19A H 0.3523 1.1135 0.0324 0.282 Uiso 1 1 calc R . .
H19B H 0.3238 0.9660 0.0260 0.282 Uiso 1 1 calc R . .
C18 C 0.3996(9) 0.9643(17) 0.0507(9) 0.382(17) Uani 1 1 d . . .
H18A H 0.4310 1.0206 0.0420 0.458 Uiso 1 1 calc R . .
H18B H 0.3937 0.9936 0.0883 0.458 Uiso 1 1 calc R . .
N20 N 0.3529(3) 1.0297(9) -0.0469(3) 0.123(2) Uani 1 1 d DU . .
C21 C 0.2983(4) 1.0949(12) -0.0729(6) 0.112(5) Uani 0.646(13) 1 d PDU A 1
H21A H 0.2881 1.1706 -0.0491 0.134 Uiso 0.646(13) 1 calc PR A 1
H21B H 0.3024 1.1341 -0.1096 0.134 Uiso 0.646(13) 1 calc PR A 1
C22 C 0.2560(4) 0.9908(13) -0.0789(7) 0.111(5) Uani 0.646(13) 1 d PDU A 1
H22A H 0.2530 0.9484 -0.0426 0.133 Uiso 0.646(13) 1 calc PR A 1
H22B H 0.2652 0.9173 -0.1043 0.133 Uiso 0.646(13) 1 calc PR A 1
C23 C 0.1964(2) 1.0654(8) -0.1044(3) 0.105(2) Uani 1 1 d DU . .
H23A H 0.1900 1.1513 -0.0843 0.126 Uiso 0.646(13) 1 calc PR A 1
H23B H 0.1944 1.0857 -0.1444 0.126 Uiso 0.646(13) 1 calc PR A 1
H23C H 0.1742 1.1513 -0.1083 0.126 Uiso 0.354(13) 1 calc PR A 2
H23D H 0.2060 1.0456 -0.1416 0.126 Uiso 0.354(13) 1 calc PR A 2
C24 C 0.3923(6) 1.1253(12) -0.0715(6) 0.179(6) Uani 1 1 d . A .
H24A H 0.3771 1.2202 -0.0731 0.214 Uiso 1 1 calc R . .
H24B H 0.4281 1.1270 -0.0467 0.214 Uiso 1 1 calc R . .
C25 C 0.4024(5) 1.0823(12) -0.1294(7) 0.187(5) Uani 1 1 d . . .
H25A H 0.3669 1.0890 -0.1545 0.224 Uiso 1 1 calc R A .
H25B H 0.4281 1.1495 -0.1425 0.224 Uiso 1 1 calc R . .
C26 C 0.4250(4) 0.9424(13) -0.1345(6) 0.180(5) Uani 1 1 d . A .
H26A H 0.3979 0.8744 -0.1244 0.215 Uiso 1 1 calc R . .
H26B H 0.4590 0.9329 -0.1074 0.215 Uiso 1 1 calc R . .
C27 C 0.4394(5) 0.9048(15) -0.1950(6) 0.203(6) Uani 1 1 d . . .
H27A H 0.4677 0.9713 -0.2036 0.244 Uiso 1 1 calc R A .
H27B H 0.4569 0.8124 -0.1925 0.244 Uiso 1 1 calc R . .
C28 C 0.3967(5) 0.9027(13) -0.2414(5) 0.182(5) Uani 1 1 d . A .
H28A H 0.4129 0.8704 -0.2740 0.219 Uiso 1 1 calc R . .
H28B H 0.3840 0.9988 -0.2490 0.219 Uiso 1 1 calc R . .
C29 C 0.3447(4) 0.8116(12) -0.2365(4) 0.155(4) Uani 1 1 d . . .
H29A H 0.3266 0.8495 -0.2060 0.186 Uiso 1 1 calc R A .
H29B H 0.3185 0.8231 -0.2710 0.186 Uiso 1 1 calc R . .
C30 C 0.3531(3) 0.6587(11) -0.2264(3) 0.123(3) Uani 1 1 d . A .
H30A H 0.3825 0.6449 -0.1945 0.147 Uiso 1 1 calc R . .
H30B H 0.3656 0.6161 -0.2592 0.147 Uiso 1 1 calc R . .
C31 C 0.2999(3) 0.5850(8) -0.2145(2) 0.092(2) Uani 1 1 d . . .
H31A H 0.2691 0.6073 -0.2441 0.110 Uiso 1 1 calc R A .
H31B H 0.3056 0.4838 -0.2143 0.110 Uiso 1 1 calc R . .
C21B C 0.2901(6) 0.9902(18) -0.0688(9) 0.080(6) Uani 0.354(13) 1 d PDU A 2
H21C H 0.2875 0.9552 -0.1071 0.096 Uiso 0.354(13) 1 calc PR A 2
H21D H 0.2784 0.9152 -0.0455 0.096 Uiso 0.354(13) 1 calc PR A 2
C22B C 0.2532(6) 1.1069(19) -0.0676(9) 0.094(7) Uani 0.354(13) 1 d PDU A 2
H22C H 0.2690 1.1901 -0.0830 0.112 Uiso 0.354(13) 1 calc PR A 2
H22D H 0.2472 1.1270 -0.0292 0.112 Uiso 0.354(13) 1 calc PR A 2
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'
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
_geom_angle_publ_flag
C7 Co1 C15 62.6(2) . . ?
C7 Co1 C16 43.2(2) . . ?
C15 Co1 C16 43.0(2) . . ?
C7 Co1 C6 43.3(2) . . ?
C15 Co1 C6 43.2(2) . . ?
C16 Co1 C6 62.8(3) . . ?
C7 Co1 C5 116.2(3) . . ?
C15 Co1 C5 160.8(3) . . ?
C16 Co1 C5 150.0(4) . . ?
C6 Co1 C5 121.4(3) . . ?
C7 Co1 C1 140.6(3) . . ?
C15 Co1 C1 127.9(3) . . ?
C16 Co1 C1 170.4(4) . . ?
C6 Co1 C1 113.4(3) . . ?
C5 Co1 C1 39.6(3) . . ?
C7 Co1 C3 143.6(4) . . ?
C15 Co1 C3 127.6(3) . . ?
C16 Co1 C3 115.7(3) . . ?
C6 Co1 C3 169.1(4) . . ?
C5 Co1 C3 66.0(3) . . ?
C1 Co1 C3 66.2(3) . . ?
C7 Co1 C4 117.6(3) . . ?
C15 Co1 C4 159.6(3) . . ?
C16 Co1 C4 121.4(3) . . ?
C6 Co1 C4 151.7(3) . . ?
C5 Co1 C4 39.5(3) . . ?
C1 Co1 C4 66.4(3) . . ?
C3 Co1 C4 39.1(3) . . ?
C7 Co1 C2 175.9(3) . . ?
C15 Co1 C2 113.4(3) . . ?
C16 Co1 C2 135.1(3) . . ?
C6 Co1 C2 133.1(4) . . ?
C5 Co1 C2 67.0(3) . . ?
C1 Co1 C2 40.2(3) . . ?
C3 Co1 C2 39.4(3) . . ?
C4 Co1 C2 66.6(3) . . ?
C5 C1 C2 108.1(8) . . ?
C5 C1 Co1 70.1(4) . . ?
C2 C1 Co1 70.5(4) . . ?
C3 C2 C1 106.1(7) . . ?
C3 C2 Co1 69.9(4) . . ?
C1 C2 Co1 69.3(4) . . ?
C4 C3 C2 109.8(8) . . ?
C4 C3 Co1 70.7(4) . . ?
C2 C3 Co1 70.7(4) . . ?
C3 C4 C5 107.6(8) . . ?
C3 C4 Co1 70.2(4) . . ?
C5 C4 Co1 69.6(4) . . ?
C1 C5 C4 108.3(7) . . ?
C1 C5 Co1 70.3(4) . . ?
C4 C5 Co1 70.8(4) . . ?
C15 C6 C7 89.3(5) . . ?
C15 C6 C23 134.0(6) . . ?
C7 C6 C23 136.0(5) . . ?
C15 C6 Co1 68.1(3) . . ?
C7 C6 Co1 67.7(3) . . ?
C23 C6 Co1 128.3(5) . . ?
C16 C7 C6 90.2(5) . . ?
C16 C7 C8 135.1(7) . . ?
C6 C7 C8 134.4(6) . . ?
C16 C7 Co1 68.7(3) . . ?
C6 C7 Co1 69.0(3) . . ?
C8 C7 Co1 124.6(4) . . ?
C16 C7 C15 44.9(4) . . ?
C6 C7 C15 45.3(3) . . ?
C8 C7 C15 176.5(4) . . ?
Co1 C7 C15 58.9(2) . . ?
C7 C8 C9 113.9(5) . . ?
C10 C9 C8 114.2(5) . . ?
N11 C10 C9 113.8(5) . . ?
C10 N11 C12 112.5(4) . . ?
C10 N11 C31 113.5(4) . . ?
C12 N11 C31 109.6(4) . . ?
N11 C12 C13 113.2(5) . . ?
C14 C13 C12 110.8(5) 7_565 . ?
C13 C14 C15 114.0(5) 7_565 . ?
C16 C15 C6 90.5(5) . . ?
C16 C15 C14 135.8(6) . . ?
C6 C15 C14 133.6(7) . . ?
C16 C15 Co1 68.4(3) . . ?
C6 C15 Co1 68.7(3) . . ?
C14 C15 Co1 123.7(4) . . ?
C16 C15 C7 45.1(4) . . ?
C6 C15 C7 45.4(3) . . ?
C14 C15 C7 177.7(4) . . ?
Co1 C15 C7 58.5(2) . . ?
C15 C16 C7 90.0(6) . . ?
C15 C16 C17 134.3(7) . . ?
C7 C16 C17 135.4(7) . . ?
C15 C16 Co1 68.6(4) . . ?
C7 C16 Co1 68.1(3) . . ?
C17 C16 Co1 125.8(5) . . ?
C18 C17 C16 125.8(13) 7_565 . ?
C18 C19 N20 123.3(15) . . ?
C17 C18 C19 136.1(17) 7_565 . ?
C24 N20 C21 98.6(8) . . ?
C24 N20 C21B 130.3(10) . . ?
C21 N20 C21B 38.8(7) . . ?
C24 N20 C19 119.2(9) . . ?
C21 N20 C19 111.6(8) . . ?
C21B N20 C19 103.6(11) . . ?
C22 C21 N20 109.0(9) . . ?
C21 C22 C23 108.3(9) . . ?
C6 C23 C22B 128.3(10) . . ?
C6 C23 C22 100.2(6) . . ?
C22B C23 C22 41.7(7) . . ?
C25 C24 N20 113.2(9) . . ?
C26 C25 C24 116.1(12) . . ?
C25 C26 C27 114.8(12) . . ?
C28 C27 C26 120.0(9) . . ?
C27 C28 C29 117.2(9) . . ?
C30 C29 C28 118.2(8) . . ?
C29 C30 C31 112.6(7) . . ?
N11 C31 C30 110.3(5) . . ?
C22B C21B N20 112.3(12) . . ?
C21B C22B C23 106.7(12) . . ?
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
Co1 C7 1.953(5) . ?
Co1 C15 1.963(5) . ?
Co1 C16 1.961(6) . ?
Co1 C6 1.972(5) . ?
Co1 C5 2.041(6) . ?
Co1 C1 2.044(7) . ?
Co1 C3 2.051(6) . ?
Co1 C4 2.056(6) . ?
Co1 C2 2.060(7) . ?
C1 C5 1.384(10) . ?
C1 C2 1.411(10) . ?
C2 C3 1.386(10) . ?
C3 C4 1.374(10) . ?
C4 C5 1.386(9) . ?
C6 C15 1.448(8) . ?
C6 C7 1.449(8) . ?
C6 C23 1.480(9) . ?
C7 C16 1.441(8) . ?
C7 C8 1.512(8) . ?
C7 C15 2.036(8) . ?
C8 C9 1.528(7) . ?
C9 C10 1.513(7) . ?
C10 N11 1.449(6) . ?
N11 C12 1.452(6) . ?
N11 C31 1.480(7) . ?
C12 C13 1.529(7) . ?
C13 C14 1.495(7) 7_565 ?
C14 C13 1.495(7) 7_565 ?
C14 C15 1.503(8) . ?
C15 C16 1.437(9) . ?
C16 C17 1.481(11) . ?
C17 C18 1.266(16) 7_565 ?
C19 C18 1.297(15) . ?
C19 N20 1.562(14) . ?
C18 C17 1.266(16) 7_565 ?
N20 C24 1.490(14) . ?
N20 C21 1.500(10) . ?
N20 C21B 1.567(15) . ?
C21 C22 1.410(12) . ?
C22 C23 1.633(11) . ?
C23 C22B 1.564(14) . ?
C24 C25 1.497(15) . ?
C25 C26 1.445(13) . ?
C26 C27 1.578(15) . ?
C27 C28 1.399(14) . ?
C28 C29 1.534(13) . ?
C29 C30 1.480(11) . ?
C30 C31 1.517(9) . ?
C21B C22B 1.421(16) . ?
