#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:54:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179268 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/88/4318819.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_4318819
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            'C81 H72 B4 F16 N12 Zn2'
_chemical_formula_weight         1691.49
_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                   10.610(2)
_cell_length_b                   10.610(2)
_cell_length_c                   41.124(11)
_cell_measurement_temperature    293(2)
_cell_volume                     4009.2(15)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            18887
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2366
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0615
_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)+(0.1360P)²+1.6900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                1860
_reflns_number_total             2366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203623_01.cif
_cod_data_source_block           complex_1
_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        4009.5(15)
_cod_database_code               4318819
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
Zn1 Zn 1.0000 1.0000 0.109690(17) 0.0511(4) Uani 1 3 d S . .
N1 N 0.8043(4) 0.8959(4) 0.07921(8) 0.0558(8) Uani 1 1 d . . .
N2 N 0.8610(4) 0.7972(4) 0.13334(7) 0.0516(8) Uani 1 1 d . . .
C1 C 0.7758(5) 0.9493(6) 0.05260(10) 0.0696(12) Uani 1 1 d . . .
H1A H 0.8359 1.0472 0.0476 0.084 Uiso 1 1 calc R . .
C2 C 0.6611(5) 0.8652(6) 0.03225(12) 0.0761(13) Uani 1 1 d . . .
H2A H 0.6431 0.9059 0.0140 0.091 Uiso 1 1 calc R . .
C3 C 0.5741(6) 0.7213(7) 0.03928(12) 0.0856(15) Uani 1 1 d . . .
H3A H 0.4983 0.6615 0.0254 0.103 Uiso 1 1 calc R . .
C4 C 0.5996(5) 0.6659(5) 0.06693(11) 0.0708(12) Uani 1 1 d . . .
H4A H 0.5397 0.5686 0.0724 0.085 Uiso 1 1 calc R . .
C5 C 0.7155(4) 0.7565(4) 0.08655(9) 0.0543(9) Uani 1 1 d . . .
C6 C 0.7498(4) 0.7047(4) 0.11753(9) 0.0528(9) Uani 1 1 d . . .
C7 C 0.6509(5) 0.5495(5) 0.12741(13) 0.0795(14) Uani 1 1 d . . .
H7A H 0.6897 0.5279 0.1463 0.119 Uiso 1 1 calc R . .
H7B H 0.6436 0.4861 0.1099 0.119 Uiso 1 1 calc R . .
H7C H 0.5561 0.5352 0.1323 0.119 Uiso 1 1 calc R . .
C10 C 0.8687(9) 0.7031(8) 0.21972(12) 0.116(3) Uani 1 1 d . . .
H10A H 0.8253 0.7037 0.2393 0.139 Uiso 1 1 calc R . .
C9 C 0.8313(8) 0.7491(7) 0.19195(11) 0.0933(19) Uani 1 1 d . . .
H9A H 0.7618 0.7781 0.1926 0.112 Uiso 1 1 calc R . .
C8 C 0.8985(5) 0.7513(4) 0.16320(9) 0.0559(10) Uani 1 1 d . . .
C13 C 1.0006(5) 0.7099(4) 0.16269(9) 0.0585(10) Uani 1 1 d . . .
H13A H 1.0477 0.7136 0.1433 0.070 Uiso 1 1 calc R . .
C12 C 1.0346(6) 0.6624(5) 0.19069(11) 0.0717(13) Uani 1 1 d . . .
H12A H 1.1044 0.6338 0.1900 0.086 Uiso 1 1 calc R . .
C11 C 0.9681(7) 0.6564(5) 0.21941(10) 0.0837(16) Uani 1 1 d . . .
C14 C 1.0000 0.5944(6) 0.2500 0.115(4) Uani 1 2 d S . .
H14A H 1.0821 0.5820 0.2457 0.138 Uiso 1 1 d R . .
B2 B 0.6667 0.3333 0.0435(2) 0.122(5) Uani 1 3 d SDU . .
F3 F 0.6667 0.3333 0.0102(3) 0.206(10) Uani 0.50 3 d SPDU A 1
F4 F 0.6951(9) 0.2285(9) 0.0566(3) 0.135(3) Uani 0.50 1 d PDU A 1
F3' F 0.6667 0.3333 0.0762(3) 0.190(8) Uani 0.50 3 d SPDU A 2
F4' F 0.607(2) 0.398(2) 0.0260(3) 0.253(8) Uani 0.50 1 d PDU A 2
B1 B 0.3333 0.6667 0.1277(3) 0.121(5) Uani 1 3 d SDU . .
F1 F 0.3333 0.6667 0.1613(4) 0.165(7) Uani 0.50 3 d SPDU B 1
F2 F 0.4583(5) 0.7847(6) 0.11365(15) 0.0825(15) Uani 0.50 1 d PDU B 1
F2' F 0.3123(15) 0.7680(13) 0.1448(3) 0.209(5) Uani 0.50 1 d PDU B 2
F1' F 0.3333 0.6667 0.0943(4) 0.301(13) Uani 0.50 3 d SPDU B 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'
F F 0.0171 0.0103 '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'
Zn Zn 0.2839 1.4301 '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 Zn1 N2 100.96(10) 2_765 3_675 ?
N2 Zn1 N2 100.96(10) 2_765 . ?
N2 Zn1 N2 100.96(10) 3_675 . ?
N2 Zn1 N1 165.55(13) 2_765 . ?
N2 Zn1 N1 93.48(13) 3_675 . ?
N2 Zn1 N1 75.54(13) . . ?
N2 Zn1 N1 93.48(13) 2_765 3_675 ?
N2 Zn1 N1 75.54(13) 3_675 3_675 ?
N2 Zn1 N1 165.55(13) . 3_675 ?
N1 Zn1 N1 90.57(13) . 3_675 ?
N2 Zn1 N1 75.54(12) 2_765 2_765 ?
N2 Zn1 N1 165.55(13) 3_675 2_765 ?
N2 Zn1 N1 93.48(13) . 2_765 ?
N1 Zn1 N1 90.57(13) . 2_765 ?
N1 Zn1 N1 90.57(13) 3_675 2_765 ?
C5 N1 C1 118.2(4) . . ?
C5 N1 Zn1 113.3(3) . . ?
C1 N1 Zn1 127.8(3) . . ?
C6 N2 C8 118.6(3) . . ?
C6 N2 Zn1 116.8(3) . . ?
C8 N2 Zn1 123.8(3) . . ?
N1 C1 C2 122.6(5) . . ?
C3 C2 C1 118.8(4) . . ?
C2 C3 C4 119.3(5) . . ?
C3 C4 C5 119.0(5) . . ?
N1 C5 C4 122.0(4) . . ?
N1 C5 C6 115.6(3) . . ?
C4 C5 C6 122.4(4) . . ?
N2 C6 C7 125.3(4) . . ?
N2 C6 C5 116.9(3) . . ?
C7 C6 C5 117.8(4) . . ?
C11 C10 C9 122.1(5) . . ?
C8 C9 C10 118.7(5) . . ?
C13 C8 C9 119.9(4) . . ?
C13 C8 N2 119.6(4) . . ?
C9 C8 N2 120.5(4) . . ?
C8 C13 C12 120.2(4) . . ?
C11 C12 C13 121.3(5) . . ?
C12 C11 C10 117.7(4) . . ?
C12 C11 C14 120.8(4) . . ?
C10 C11 C14 121.5(4) . . ?
C11 C14 C11 114.7(5) 6_765 . ?
F3' B2 F4' 122.1(6) . 3_665 ?
F3' B2 F4' 122.1(6) . 2_655 ?
F4' B2 F4' 94.4(8) 3_665 2_655 ?
F3' B2 F4' 122.1(6) . . ?
F4' B2 F4' 94.4(8) 3_665 . ?
F4' B2 F4' 94.4(8) 2_655 . ?
F3' B2 F3 180.000(1) . . ?
F4' B2 F3 57.9(6) 3_665 . ?
F4' B2 F3 57.9(6) 2_655 . ?
F4' B2 F3 57.9(6) . . ?
F3' B2 F4 67.3(5) . . ?
F4' B2 F4 91.6(9) 3_665 . ?
F4' B2 F4 68.6(8) 2_655 . ?
F4' B2 F4 162.4(9) . . ?
F3 B2 F4 112.7(5) . . ?
F3' B2 F4 67.3(5) . 2_655 ?
F4' B2 F4 68.6(8) 3_665 2_655 ?
F4' B2 F4 162.4(9) 2_655 2_655 ?
F4' B2 F4 91.6(9) . 2_655 ?
F3 B2 F4 112.7(5) . 2_655 ?
F4 B2 F4 106.0(6) . 2_655 ?
F3' B2 F4 67.3(5) . 3_665 ?
F4' B2 F4 162.4(9) 3_665 3_665 ?
F4' B2 F4 91.6(9) 2_655 3_665 ?
F4' B2 F4 68.6(8) . 3_665 ?
F3 B2 F4 112.7(5) . 3_665 ?
F4 B2 F4 106.0(6) . 3_665 ?
F4 B2 F4 106.0(6) 2_655 3_665 ?
F1' B1 F1 180.000(2) . . ?
F1' B1 F2' 120.2(7) . . ?
F1 B1 F2' 59.8(7) . . ?
F1' B1 F2' 120.2(7) . 2_665 ?
F1 B1 F2' 59.8(7) . 2_665 ?
F2' B1 F2' 96.9(10) . 2_665 ?
F1' B1 F2' 120.2(7) . 3_565 ?
F1 B1 F2' 59.8(7) . 3_565 ?
F2' B1 F2' 96.9(10) . 3_565 ?
F2' B1 F2' 96.9(10) 2_665 3_565 ?
F1' B1 F2 65.8(5) . 2_665 ?
F1 B1 F2 114.2(5) . 2_665 ?
F2' B1 F2 71.2(6) . 2_665 ?
F2' B1 F2 87.9(6) 2_665 2_665 ?
F2' B1 F2 167.7(8) 3_565 2_665 ?
F1' B1 F2 65.8(5) . . ?
F1 B1 F2 114.2(5) . . ?
F2' B1 F2 87.9(6) . . ?
F2' B1 F2 167.7(8) 2_665 . ?
F2' B1 F2 71.2(6) 3_565 . ?
F2 B1 F2 104.4(6) 2_665 . ?
F1' B1 F2 65.8(5) . 3_565 ?
F1 B1 F2 114.2(5) . 3_565 ?
F2' B1 F2 167.7(8) . 3_565 ?
F2' B1 F2 71.2(6) 2_665 3_565 ?
F2' B1 F2 87.9(6) 3_565 3_565 ?
F2 B1 F2 104.4(6) 2_665 3_565 ?
F2 B1 F2 104.4(6) . 3_565 ?
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
Zn1 N2 2.140(3) 2_765 ?
Zn1 N2 2.140(3) 3_675 ?
Zn1 N2 2.140(3) . ?
Zn1 N1 2.193(3) . ?
Zn1 N1 2.193(3) 3_675 ?
Zn1 N1 2.193(3) 2_765 ?
N1 C5 1.331(5) . ?
N1 C1 1.335(5) . ?
N2 C6 1.273(5) . ?
N2 C8 1.448(5) . ?
C1 C2 1.376(6) . ?
C2 C3 1.363(7) . ?
C3 C4 1.367(7) . ?
C4 C5 1.380(6) . ?
C5 C6 1.503(6) . ?
C6 C7 1.500(6) . ?
C10 C11 1.371(8) . ?
C10 C9 1.376(7) . ?
C9 C8 1.375(6) . ?
C8 C13 1.357(6) . ?
C13 C12 1.376(6) . ?
C12 C11 1.361(7) . ?
C11 C14 1.534(5) . ?
C14 C11 1.534(5) 6_765 ?
B2 F3' 1.344(9) . ?
B2 F4' 1.354(8) 3_665 ?
B2 F4' 1.354(8) 2_655 ?
B2 F4' 1.354(8) . ?
B2 F3 1.369(9) . ?
B2 F4 1.398(6) . ?
B2 F4 1.398(6) 2_655 ?
B2 F4 1.398(6) 3_665 ?
B1 F1' 1.374(9) . ?
B1 F1 1.381(9) . ?
B1 F2' 1.392(8) . ?
B1 F2' 1.392(8) 2_665 ?
B1 F2' 1.392(8) 3_565 ?
B1 F2 1.415(6) 2_665 ?
B1 F2 1.415(6) . ?
B1 F2 1.415(6) 3_565 ?
