#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:54:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179268 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/88/4318821.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_4318821
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 Mn2 N12'
_chemical_formula_weight         1670.63
_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                   10.6848(15)
_cell_length_b                   10.6848(15)
_cell_length_c                   41.052(8)
_cell_measurement_temperature    293(2)
_cell_volume                     4058.8(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       9
_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       -43
_diffrn_reflns_number            19022
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0672
_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)+(0.1150P)²+1.9319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2100
_reflns_number_gt                1637
_reflns_number_total             2401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0203623_03.cif
_cod_data_source_block           complex_3
_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_database_code               4318821
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
Mn1 Mn 1.0000 1.0000 0.11010(3) 0.0576(4) Uani 1 3 d S . .
N1 N 1.2015(4) 1.0900(4) 0.07899(8) 0.0638(10) Uani 1 1 d . . .
N2 N 1.1475(4) 0.9371(4) 0.13344(8) 0.0584(9) Uani 1 1 d . . .
C1 C 1.2291(6) 1.1703(6) 0.05195(12) 0.0826(15) Uani 1 1 d . . .
H1A H 1.1684 1.2064 0.0468 0.099 Uiso 1 1 calc R . .
C2 C 1.3429(6) 1.2014(6) 0.03160(13) 0.0862(16) Uani 1 1 d . . .
H2A H 1.3604 1.2596 0.0134 0.103 Uiso 1 1 calc R . .
C3 C 1.4297(6) 1.1456(7) 0.03859(13) 0.0942(18) Uani 1 1 d . . .
H3A H 1.5046 1.1610 0.0246 0.113 Uiso 1 1 calc R . .
C4 C 1.4052(6) 1.0653(7) 0.06685(13) 0.0835(15) Uani 1 1 d . . .
H4A H 1.4653 1.0290 0.0725 0.100 Uiso 1 1 calc R . .
C5 C 1.2901(5) 1.0405(5) 0.08626(11) 0.0602(11) Uani 1 1 d . . .
C6 C 1.2580(5) 0.9554(5) 0.11741(11) 0.0603(11) Uani 1 1 d . . .
C7 C 1.3575(6) 0.9021(7) 0.12714(14) 0.0876(16) Uani 1 1 d . . .
H7A H 1.3267 0.8525 0.1476 0.131 Uiso 1 1 calc R . .
H7B H 1.4539 0.9826 0.1292 0.131 Uiso 1 1 calc R . .
H7C H 1.3559 0.8370 0.1108 0.131 Uiso 1 1 calc R . .
C8 C 1.1107(6) 0.8558(5) 0.16323(10) 0.0651(12) Uani 1 1 d . . .
C9 C 1.1754(9) 0.9180(7) 0.19199(13) 0.121(3) Uani 1 1 d . . .
H9A H 1.2456 1.0153 0.1928 0.145 Uiso 1 1 calc R . .
C10 C 1.1355(12) 0.8348(8) 0.22016(14) 0.146(4) Uani 1 1 d . . .
H10A H 1.1787 0.8778 0.2398 0.175 Uiso 1 1 calc R . .
C11 C 1.0330(9) 0.6896(6) 0.21958(13) 0.103(2) Uani 1 1 d . . .
C12 C 0.9701(7) 0.6330(6) 0.19104(13) 0.0813(15) Uani 1 1 d . . .
H12A H 0.9007 0.5355 0.1901 0.098 Uiso 1 1 calc R . .
C13 C 1.0042(6) 0.7139(5) 0.16292(11) 0.0686(13) Uani 1 1 d . . .
H13A H 0.9548 0.6719 0.1437 0.082 Uiso 1 1 calc R . .
C14 C 1.0000 0.5982(8) 0.2500 0.150(6) Uani 1 2 d S . .
H14A H 1.0812 0.5856 0.2545 0.180 Uiso 1 1 d R . .
B1 B 0.6667 0.3333 0.1286(3) 0.129(5) Uani 1 3 d SDU . .
F1 F 0.7788(7) 0.4555(6) 0.11530(18) 0.0948(19) Uani 0.50 1 d PDU A 1
F2 F 0.6667 0.3333 0.1608(3) 0.155(6) Uani 0.50 3 d SPDU A 1
F1' F 0.6966(15) 0.4550(11) 0.1435(3) 0.219(6) Uani 0.50 1 d PDU A 2
F2' F 0.6667 0.3333 0.0968(4) 0.293(12) Uani 0.50 3 d SPDU A 2
B2 B 0.3333 0.6667 0.04465(19) 0.128(5) Uani 1 3 d SDU . .
F3' F 0.4384(19) 0.7790(17) 0.0309(3) 0.314(10) Uani 0.50 1 d PDU B 1
F4' F 0.3333 0.6667 0.0761(2) 0.192(8) Uani 0.50 3 d SPDU B 1
F3 F 0.4591(9) 0.7665(9) 0.0584(2) 0.131(3) Uani 0.50 1 d PDU B 2
F4 F 0.3333 0.6667 0.0129(2) 0.181(8) 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'
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'
Mn Mn 0.3368 0.7283 '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 Mn1 N2 102.69(11) . 2_765 ?
N2 Mn1 N2 102.69(11) . 3_675 ?
N2 Mn1 N2 102.69(11) 2_765 3_675 ?
N2 Mn1 N1 94.10(14) . 3_675 ?
N2 Mn1 N1 163.21(14) 2_765 3_675 ?
N2 Mn1 N1 72.73(13) 3_675 3_675 ?
N2 Mn1 N1 163.21(14) . 2_765 ?
N2 Mn1 N1 72.73(13) 2_765 2_765 ?
N2 Mn1 N1 94.10(14) 3_675 2_765 ?
N1 Mn1 N1 91.28(13) 3_675 2_765 ?
N2 Mn1 N1 72.73(13) . . ?
N2 Mn1 N1 94.10(14) 2_765 . ?
N2 Mn1 N1 163.21(14) 3_675 . ?
N1 Mn1 N1 91.28(13) 3_675 . ?
N1 Mn1 N1 91.28(13) 2_765 . ?
C5 N1 C1 117.9(4) . . ?
C5 N1 Mn1 114.8(3) . . ?
C1 N1 Mn1 126.6(3) . . ?
C6 N2 C8 118.9(4) . . ?
C6 N2 Mn1 118.2(3) . . ?
C8 N2 Mn1 122.0(3) . . ?
N1 C1 C2 122.9(5) . . ?
C3 C2 C1 118.8(5) . . ?
C2 C3 C4 119.2(5) . . ?
C5 C4 C3 118.5(5) . . ?
N1 C5 C4 122.7(4) . . ?
N1 C5 C6 116.0(4) . . ?
C4 C5 C6 121.3(4) . . ?
N2 C6 C7 125.8(4) . . ?
N2 C6 C5 116.3(4) . . ?
C7 C6 C5 117.9(4) . . ?
C9 C8 C13 119.1(5) . . ?
C9 C8 N2 121.6(5) . . ?
C13 C8 N2 119.2(4) . . ?
C8 C9 C10 119.4(6) . . ?
C11 C10 C9 121.5(6) . . ?
C12 C11 C10 117.4(5) . . ?
C12 C11 C14 122.0(6) . . ?
C10 C11 C14 120.5(6) . . ?
C11 C12 C13 122.4(6) . . ?
C8 C13 C12 120.0(5) . . ?
C11 C14 C11 116.2(6) . 6_765 ?
F2' B1 F2 180.000(1) . . ?
F2' B1 F1' 117.6(7) . 3_665 ?
F2 B1 F1' 62.4(7) . 3_665 ?
F2' B1 F1' 117.6(7) . 2_655 ?
F2 B1 F1' 62.4(7) . 2_655 ?
F1' B1 F1' 100.3(9) 3_665 2_655 ?
F2' B1 F1' 117.6(7) . . ?
F2 B1 F1' 62.4(7) . . ?
F1' B1 F1' 100.3(9) 3_665 . ?
F1' B1 F1' 100.3(9) 2_655 . ?
F2' B1 F1 66.5(5) . 3_665 ?
F2 B1 F1 113.5(5) . 3_665 ?
F1' B1 F1 65.2(7) 3_665 3_665 ?
F1' B1 F1 90.8(6) 2_655 3_665 ?
F1' B1 F1 163.4(6) . 3_665 ?
F2' B1 F1 66.5(5) . . ?
F2 B1 F1 113.5(5) . . ?
F1' B1 F1 90.8(6) 3_665 . ?
F1' B1 F1 163.4(6) 2_655 . ?
F1' B1 F1 65.2(7) . . ?
F1 B1 F1 105.2(6) 3_665 . ?
F2' B1 F1 66.5(5) . 2_655 ?
F2 B1 F1 113.5(5) . 2_655 ?
F1' B1 F1 163.4(6) 3_665 2_655 ?
F1' B1 F1 65.2(7) 2_655 2_655 ?
F1' B1 F1 90.8(6) . 2_655 ?
F1 B1 F1 105.2(6) 3_665 2_655 ?
F1 B1 F1 105.2(6) . 2_655 ?
F4' B2 F3' 115.8(7) . 2_665 ?
F4' B2 F3' 115.8(7) . . ?
F3' B2 F3' 102.4(8) 2_665 . ?
F4' B2 F3' 115.8(7) . 3_565 ?
F3' B2 F3' 102.4(8) 2_665 3_565 ?
F3' B2 F3' 102.4(8) . 3_565 ?
F4' B2 F4 180.000(1) . . ?
F3' B2 F4 64.2(7) 2_665 . ?
F3' B2 F4 64.2(7) . . ?
F3' B2 F4 64.2(7) 3_565 . ?
F4' B2 F3 65.4(5) . 2_665 ?
F3' B2 F3 52.4(8) 2_665 2_665 ?
F3' B2 F3 113.5(13) . 2_665 ?
F3' B2 F3 139.1(14) 3_565 2_665 ?
F4 B2 F3 114.6(5) . 2_665 ?
F4' B2 F3 65.4(5) . . ?
F3' B2 F3 139.1(13) 2_665 . ?
F3' B2 F3 52.4(8) . . ?
F3' B2 F3 113.5(13) 3_565 . ?
F4 B2 F3 114.6(5) . . ?
F3 B2 F3 103.9(6) 2_665 . ?
F4' B2 F3 65.4(5) . 3_565 ?
F3' B2 F3 113.5(13) 2_665 3_565 ?
F3' B2 F3 139.1(13) . 3_565 ?
F3' B2 F3 52.4(8) 3_565 3_565 ?
F4 B2 F3 114.6(5) . 3_565 ?
F3 B2 F3 103.9(6) 2_665 3_565 ?
F3 B2 F3 103.9(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
Mn1 N2 2.216(4) . ?
Mn1 N2 2.216(4) 2_765 ?
Mn1 N2 2.216(4) 3_675 ?
Mn1 N1 2.263(4) 3_675 ?
Mn1 N1 2.263(4) 2_765 ?
Mn1 N1 2.263(4) . ?
N1 C5 1.328(6) . ?
N1 C1 1.342(6) . ?
N2 C6 1.278(6) . ?
N2 C8 1.436(5) . ?
C1 C2 1.372(7) . ?
C2 C3 1.361(8) . ?
C3 C4 1.388(8) . ?
C4 C5 1.376(7) . ?
C5 C6 1.506(6) . ?
C6 C7 1.490(7) . ?
C8 C9 1.362(7) . ?
C8 C13 1.368(7) . ?
C9 C10 1.390(8) . ?
C10 C11 1.381(10) . ?
C11 C12 1.335(8) . ?
C11 C14 1.514(6) . ?
C12 C13 1.377(7) . ?
C14 C11 1.514(6) 6_765 ?
B1 F2' 1.307(9) . ?
B1 F2 1.322(9) . ?
B1 F1' 1.323(7) 3_665 ?
B1 F1' 1.323(7) 2_655 ?
B1 F1' 1.323(7) . ?
B1 F1 1.368(6) 3_665 ?
B1 F1 1.368(6) . ?
B1 F1 1.368(6) 2_655 ?
B2 F4' 1.291(9) . ?
B2 F3' 1.293(8) 2_665 ?
B2 F3' 1.293(8) . ?
B2 F3' 1.293(8) 3_565 ?
B2 F4 1.303(8) . ?
B2 F3 1.352(7) 2_665 ?
B2 F3 1.352(7) . ?
B2 F3 1.352(6) 3_565 ?
