#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:54:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179268 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/88/4318822.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_4318822
loop_
_publ_author_name
'Guo Dong'
'Pang Ke-liang'
'Duan Chun-ying'
'He Cheng'
'Meng Qing-jin'
_publ_contact_author_address
;
Coordination Chemistry Institute
The State Key Laboratory of Coordinaiton Chemistry
Nanjing University , Nanjing 210093
P. R. China
;
_publ_contact_author_email       duancy@nju.edu.cn
_publ_contact_author_fax         '00 86 25 331 4502'
_publ_contact_author_name        'Dr. Duan Chun-ying'
_publ_contact_author_phone       '00 86 25 359 7006'
_publ_section_title
;
 Design and Crystal Structures of Triple Helicates with Crystallographic
 Idealized D3 Symmetry: The Role of Side Chain Effect on Crystal Packing
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5978
_journal_page_last               5985
_journal_paper_doi               10.1021/ic0203623
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C78 H66 B4 Co2 F16 N12 O3'
_chemical_formula_weight         1684.53
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.5469(8)
_cell_length_b                   10.5469(8)
_cell_length_c                   40.909(4)
_cell_measurement_reflns_used    1714
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.64
_cell_measurement_theta_min      2.54
_cell_volume                     3940.9(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0862
_diffrn_reflns_av_sigmaI/netI    0.0973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            18742
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2332
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.0729
_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)+(0.0750P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1947
_reflns_number_gt                1145
_reflns_number_total             2332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203623_04.cif
_cod_data_source_block           complex_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3941.0(6)
_cod_database_code               4318822
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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 1.0000 1.0000 0.39088(3) 0.0511(5) Uani 1 3 d S . .
N1 N 0.9012(6) 0.8069(5) 0.42004(10) 0.0546(13) Uani 1 1 d . . .
N2 N 0.7987(5) 0.8643(5) 0.36742(11) 0.0508(14) Uani 1 1 d . . .
C1 C 0.9546(8) 0.7766(8) 0.44625(17) 0.073(2) Uani 1 1 d . . .
H1A H 1.0534 0.8371 0.4510 0.087 Uiso 1 1 calc R . .
C2 C 0.8729(9) 0.6609(9) 0.46699(16) 0.081(2) Uani 1 1 d . . .
H2A H 0.9155 0.6429 0.4850 0.097 Uiso 1 1 calc R . .
C3 C 0.7281(9) 0.5737(8) 0.46028(18) 0.084(2) Uani 1 1 d . . .
H3A H 0.6685 0.4963 0.4740 0.100 Uiso 1 1 calc R . .
C4 C 0.6719(8) 0.6018(8) 0.43313(17) 0.071(2) Uani 1 1 d . . .
H4A H 0.5732 0.5431 0.4281 0.085 Uiso 1 1 calc R . .
C5 C 0.7612(7) 0.7173(7) 0.41318(14) 0.0523(16) Uani 1 1 d . . .
C6 C 0.7073(7) 0.7510(7) 0.38275(15) 0.0557(17) Uani 1 1 d . . .
C7 C 0.5530(7) 0.6525(8) 0.37222(17) 0.084(2) Uani 1 1 d . . .
H7A H 0.5330 0.6920 0.3530 0.125 Uiso 1 1 calc R . .
H7B H 0.4877 0.6448 0.3895 0.125 Uiso 1 1 calc R . .
H7C H 0.5388 0.5572 0.3674 0.125 Uiso 1 1 calc R . .
C8 C 0.7530(7) 0.9018(7) 0.33744(14) 0.0561(17) Uani 1 1 d U . .
C9 C 0.7107(7) 1.0026(7) 0.33773(15) 0.0591(17) Uani 1 1 d U . .
H9A H 0.7137 1.0543 0.3564 0.071 Uiso 1 1 calc R A 1
C10 C 0.661(6) 1.023(5) 0.3071(10) 0.058(7) Uani 0.50 1 d PU . 1
H10A H 0.6346 1.0948 0.3060 0.070 Uiso 0.50 1 calc PR . 1
C11 C 0.650(4) 0.949(3) 0.2796(9) 0.058(5) Uani 0.50 1 d PU . 1
C12 C 0.680(2) 0.841(2) 0.2815(6) 0.070(5) Uani 0.50 1 d PU . 1
H12A H 0.6670 0.7851 0.2628 0.084 Uiso 0.50 1 calc PR . 1
C13 C 0.730(3) 0.806(3) 0.3105(7) 0.080(6) Uani 0.50 1 d PU . 1
H13A H 0.7459 0.7268 0.3119 0.096 Uiso 0.50 1 calc PR . 1
C10' C 0.664(6) 1.049(5) 0.3125(10) 0.060(6) Uani 0.50 1 d PU . 2
H10B H 0.6265 1.1126 0.3133 0.072 Uiso 0.50 1 d PR . 2
C11' C 0.666(4) 0.996(3) 0.2827(10) 0.065(6) Uani 0.50 1 d PU . 2
C12' C 0.730(2) 0.907(2) 0.2791(6) 0.074(5) Uani 0.50 1 d PU . 2
H12B H 0.7479 0.8808 0.2587 0.089 Uiso 0.50 1 d PR . 2
C13' C 0.771(2) 0.859(2) 0.3073(6) 0.058(5) Uani 0.50 1 d PU . 2
H13B H 0.8204 0.8066 0.3056 0.069 Uiso 0.50 1 d PR . 2
O1 O 0.6105(13) 1.0438(16) 0.2513(7) 0.125(6) Uani 0.50 1 d PU . .
B2 B 0.3333 0.6667 0.4555(3) 0.159(6) Uani 1 3 d SDU . .
F21 F 0.3333 0.6667 0.4872(4) 0.186(7) Uani 0.50 3 d SPDU B 1
F22 F 0.4640(10) 0.7679(11) 0.4436(3) 0.142(4) Uani 0.50 1 d PDU B 1
F21' F 0.3333 0.6667 0.4242(4) 0.179(7) Uani 0.50 3 d SPDU B 2
F22' F 0.396(2) 0.7872(12) 0.4722(3) 0.240(7) Uani 0.50 1 d PDU B 2
B1 B 0.6667 0.3333 0.3718(4) 0.154(6) Uani 1 3 d SDU . .
F11 F 0.6667 0.3333 0.3379(4) 0.163(7) Uani 0.50 3 d SPDU C 1
F12 F 0.7863(8) 0.4564(8) 0.38681(18) 0.078(2) Uani 0.50 1 d PDU C 1
F11' F 0.6667 0.3333 0.4054(5) 0.231(8) Uani 0.50 3 d SPDU C 2
F12' F 0.5482(13) 0.2292(14) 0.3542(4) 0.203(5) Uani 0.50 1 d PDU C 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'
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'
O O 0.0106 0.0060 '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'
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
N2 Co1 N2 100.87(16) . 3_675 ?
N2 Co1 N2 100.87(16) . 2_765 ?
N2 Co1 N2 100.87(17) 3_675 2_765 ?
N2 Co1 N1 167.5(2) . 2_765 ?
N2 Co1 N1 91.67(19) 3_675 2_765 ?
N2 Co1 N1 76.1(2) 2_765 2_765 ?
N2 Co1 N1 76.1(2) . . ?
N2 Co1 N1 167.5(2) 3_675 . ?
N2 Co1 N1 91.67(19) 2_765 . ?
N1 Co1 N1 91.68(17) 2_765 . ?
N2 Co1 N1 91.67(19) . 3_675 ?
N2 Co1 N1 76.1(2) 3_675 3_675 ?
N2 Co1 N1 167.5(2) 2_765 3_675 ?
N1 Co1 N1 91.68(17) 2_765 3_675 ?
N1 Co1 N1 91.68(17) . 3_675 ?
C1 N1 C5 117.2(5) . . ?
C1 N1 Co1 128.4(5) . . ?
C5 N1 Co1 113.7(4) . . ?
C6 N2 C8 118.6(5) . . ?
C6 N2 Co1 116.7(4) . . ?
C8 N2 Co1 124.2(4) . . ?
N1 C1 C2 124.0(7) . . ?
C3 C2 C1 117.9(7) . . ?
C4 C3 C2 118.8(7) . . ?
C3 C4 C5 119.9(7) . . ?
N1 C5 C4 122.1(6) . . ?
N1 C5 C6 115.5(6) . . ?
C4 C5 C6 122.4(7) . . ?
N2 C6 C5 116.1(6) . . ?
N2 C6 C7 124.5(6) . . ?
C5 C6 C7 119.4(6) . . ?
C9 C8 C13' 115.4(11) . . ?
C9 C8 C13 124.0(14) . . ?
C13' C8 C13 21.6(14) . . ?
C9 C8 N2 119.8(5) . . ?
C13' C8 N2 124.0(12) . . ?
C13 C8 N2 115.0(14) . . ?
C10' C9 C8 128(2) . . ?
C10' C9 C10 14(3) . . ?
C8 C9 C10 114.0(19) . . ?
C11 C10 C9 126(4) . . ?
C12 C11 C10 118(3) . . ?
C12 C11 O1 118(2) . 5_675 ?
C10 C11 O1 123(3) . 5_675 ?
C12 C11 O1 140(3) . . ?
C10 C11 O1 102(3) . . ?
O1 C11 O1 28.1(13) 5_675 . ?
C11 C12 C13 123(2) . . ?
C12 C13 C8 114(2) . . ?
C9 C10' C11' 117(4) . . ?
C10' C11' C12' 119(3) . . ?
C10' C11' O1 120(3) . . ?
C12' C11' O1 120(3) . . ?
C10' C11' O1 136(4) . 5_675 ?
C12' C11' O1 101(2) . 5_675 ?
O1 C11' O1 28.5(13) . 5_675 ?
C13' C12' C11' 119(2) . . ?
C8 C13' C12' 120.1(19) . . ?
O1 O1 C11 86(4) 5_675 5_675 ?
O1 O1 C11' 80(4) 5_675 . ?
C11 O1 C11' 110.8(10) 5_675 . ?
O1 O1 C11' 71(3) 5_675 5_675 ?
C11 O1 C11' 15.5(18) 5_675 5_675 ?
C11' O1 C11' 110(3) . 5_675 ?
O1 O1 C11 66(3) 5_675 . ?
C11 O1 C11 105(3) 5_675 . ?
C11' O1 C11 15.1(17) . . ?
C11' O1 C11 100.8(12) 5_675 . ?
F21' B2 F22' 121.8(7) . . ?
F21' B2 F22' 121.8(7) . 2_665 ?
F22' B2 F22' 94.8(10) . 2_665 ?
F21' B2 F22' 121.8(7) . 3_565 ?
F22' B2 F22' 94.8(10) . 3_565 ?
F22' B2 F22' 94.8(10) 2_665 3_565 ?
F21' B2 F21 180.000(5) . . ?
F22' B2 F21 58.2(7) . . ?
F22' B2 F21 58.2(7) 2_665 . ?
F22' B2 F21 58.2(7) 3_565 . ?
F21' B2 F22 68.9(7) . 2_665 ?
F22' B2 F22 92.1(12) . 2_665 ?
F22' B2 F22 66.0(8) 2_665 2_665 ?
F22' B2 F22 160.1(13) 3_565 2_665 ?
F21 B2 F22 111.1(7) . 2_665 ?
F21' B2 F22 68.9(7) . . ?
F22' B2 F22 66.0(8) . . ?
F22' B2 F22 160.1(12) 2_665 . ?
F22' B2 F22 92.1(12) 3_565 . ?
F21 B2 F22 111.1(7) . . ?
F22 B2 F22 107.7(7) 2_665 . ?
F21' B2 F22 68.9(7) . 3_565 ?
F22' B2 F22 160.1(12) . 3_565 ?
F22' B2 F22 92.1(12) 2_665 3_565 ?
F22' B2 F22 66.0(9) 3_565 3_565 ?
F21 B2 F22 111.1(7) . 3_565 ?
F22 B2 F22 107.7(7) 2_665 3_565 ?
F22 B2 F22 107.7(7) . 3_565 ?
F11' B1 F12' 121.4(8) . 2_655 ?
F11' B1 F12' 121.4(8) . . ?
F12' B1 F12' 95.4(11) 2_655 . ?
F11' B1 F12' 121.4(8) . 3_665 ?
F12' B1 F12' 95.4(11) 2_655 3_665 ?
F12' B1 F12' 95.4(11) . 3_665 ?
F11' B1 F11 180.000(4) . . ?
F12' B1 F11 58.6(8) 2_655 . ?
F12' B1 F11 58.6(8) . . ?
F12' B1 F11 58.6(8) 3_665 . ?
F11' B1 F12 64.4(6) . 3_665 ?
F12' B1 F12 75.7(7) 2_655 3_665 ?
F12' B1 F12 86.1(6) . 3_665 ?
F12' B1 F12 171.1(10) 3_665 3_665 ?
F11 B1 F12 115.6(6) . 3_665 ?
F11' B1 F12 64.4(6) . . ?
F12' B1 F12 86.1(6) 2_655 . ?
F12' B1 F12 171.1(10) . . ?
F12' B1 F12 75.7(7) 3_665 . ?
F11 B1 F12 115.6(6) . . ?
F12 B1 F12 102.7(7) 3_665 . ?
F11' B1 F12 64.4(6) . 2_655 ?
F12' B1 F12 171.1(10) 2_655 2_655 ?
F12' B1 F12 75.7(7) . 2_655 ?
F12' B1 F12 86.1(6) 3_665 2_655 ?
F11 B1 F12 115.6(6) . 2_655 ?
F12 B1 F12 102.7(7) 3_665 2_655 ?
F12 B1 F12 102.7(7) . 2_655 ?
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 N2 2.106(5) . ?
Co1 N2 2.106(5) 3_675 ?
Co1 N2 2.106(5) 2_765 ?
Co1 N1 2.129(5) 2_765 ?
Co1 N1 2.129(5) . ?
Co1 N1 2.129(5) 3_675 ?
N1 C1 1.323(7) . ?
N1 C5 1.326(7) . ?
N2 C6 1.265(7) . ?
N2 C8 1.443(7) . ?
C1 C2 1.379(9) . ?
C2 C3 1.360(9) . ?
C3 C4 1.359(9) . ?
C4 C5 1.374(8) . ?
C5 C6 1.484(8) . ?
C6 C7 1.491(8) . ?
C8 C9 1.343(8) . ?
C8 C13' 1.36(3) . ?
C8 C13 1.43(3) . ?
C9 C10' 1.34(6) . ?
C9 C10 1.41(5) . ?
C10 C11 1.34(4) . ?
C11 C12 1.33(4) . ?
C11 O1 1.56(4) 5_675 ?
C11 O1 1.71(5) . ?
C12 C13 1.42(3) . ?
C10' C11' 1.35(4) . ?
C11' C12' 1.40(4) . ?
C11' O1 1.60(4) . ?
C11' O1 1.67(5) 5_675 ?
C12' C13' 1.41(3) . ?
O1 O1 0.81(3) 5_675 ?
O1 C11 1.56(4) 5_675 ?
O1 C11' 1.67(5) 5_675 ?
B2 F21' 1.280(9) . ?
B2 F22' 1.296(9) . ?
B2 F22' 1.296(8) 2_665 ?
B2 F22' 1.296(9) 3_565 ?
B2 F21 1.298(10) . ?
B2 F22 1.343(8) 2_665 ?
B2 F22 1.343(8) . ?
B2 F22 1.343(8) 3_565 ?
B1 F11' 1.375(10) . ?
B1 F12' 1.383(9) 2_655 ?
B1 F12' 1.383(9) . ?
B1 F12' 1.383(9) 3_665 ?
B1 F11 1.390(10) . ?
B1 F12 1.419(7) 3_665 ?
B1 F12 1.419(7) . ?
B1 F12 1.419(7) 2_655 ?
