#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/40/7104029.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_7104029
loop_
_publ_author_name
'Dolomanov, Oleg V'
'Blake, Alexander J'
'Champness, Neil R'
'Schröder, Martin'
'Wilson, Claire'
_publ_section_title
;
 A novel synthetic strategy for hexanuclear supramolecular
 architectures
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              682
_journal_page_last               683
_journal_paper_doi               10.1039/b300605k
_journal_year                    2003
_chemical_formula_sum            'C30 H28 B Cu F4 N6 O2'
_chemical_formula_weight         654.93
_chemical_name_common
;
bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl cupper(I) 
tetrafluoroborate hexamer
;
_chemical_name_systematic
;
bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl cupper(I)
tetrafluoroborate hexamer
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   20.467(2)
_cell_length_b                   20.467(2)
_cell_length_c                   40.139(6)
_cell_measurement_reflns_used    4997
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      2.35
_cell_volume                     14561(3)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'OLEX (Dolomanov, 2001)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.086
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            30887
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             6048
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.01
_refine_diff_density_min         -0.46
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         7646
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[σ²(Fo²)+(0.158P)²] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2416
_reflns_number_gt                3221
_reflns_number_total             7646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300605k.txt
_cod_data_source_block           Compund_1(PYYNCU)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (4
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (12 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geometrically placed' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7104029
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Cu1 Cu 0.74946(3) 0.63369(3) 0.251095(14) 0.0630(2) Uani 1 1 d . . .
N1 N 0.8326(2) 0.68996(18) 0.21603(8) 0.0544(9) Uani 1 1 d . . .
C2 C 0.8385(3) 0.7550(2) 0.20454(10) 0.0546(11) Uani 1 1 d . . .
C3 C 0.8982(3) 0.8050(2) 0.18445(11) 0.0613(12) Uani 1 1 d . . .
H3A H 0.9010 0.8501 0.1767 0.074 Uiso 1 1 calc R . .
C4 C 0.9544(3) 0.7877(2) 0.17579(12) 0.0673(13) Uani 1 1 d . . .
H4A H 0.9958 0.8211 0.1622 0.081 Uiso 1 1 calc R . .
C5 C 0.9488(3) 0.7225(2) 0.18707(12) 0.0641(12) Uani 1 1 d . . .
H5 H 0.9860 0.7094 0.1816 0.077 Uiso 1 1 calc R . .
C6 C 0.8869(3) 0.6749(2) 0.20704(11) 0.0551(11) Uani 1 1 d . . .
C7 C 0.8783(3) 0.6032(3) 0.21945(12) 0.0664(13) Uani 1 1 d . . .
C8 C 0.8758(3) 0.5466(3) 0.22644(13) 0.0657(13) Uani 1 1 d . . .
C9 C 0.8786(3) 0.4792(2) 0.23369(11) 0.0597(12) Uani 1 1 d . . .
C10 C 0.8230(3) 0.4209(3) 0.25345(13) 0.0664(13) Uani 1 1 d . . .
H10A H 0.7843 0.4264 0.2638 0.080 Uiso 1 1 calc R . .
C11 C 0.8262(3) 0.3563(3) 0.25743(12) 0.0632(12) Uani 1 1 d . . .
H11A H 0.7878 0.3168 0.2703 0.076 Uiso 1 1 calc R . .
N12 N 0.8797(2) 0.3449(2) 0.24445(9) 0.0553(9) Uani 1 1 d . . .
C13 C 0.9328(3) 0.4010(3) 0.22615(12) 0.0648(12) Uani 1 1 d . . .
H13A H 0.9711 0.3937 0.2166 0.078 Uiso 1 1 calc R . .
C14 C 0.9358(3) 0.4684(3) 0.22016(12) 0.0633(12) Uani 1 1 d . . .
H14A H 0.9753 0.5067 0.2073 0.076 Uiso 1 1 calc R . .
N1' N 0.7293(2) 0.7225(2) 0.23891(9) 0.0621(10) Uani 1 1 d . . .
C2' C 0.7765(3) 0.7688(3) 0.21445(11) 0.0599(11) Uani 1 1 d . . .
C3' C 0.7639(3) 0.8237(3) 0.19897(14) 0.0781(15) Uani 1 1 d . . .
H3'A H 0.7964 0.8544 0.1816 0.094 Uiso 1 1 calc R . .
C4' C 0.7054(4) 0.8321(3) 0.20903(15) 0.0930(18) Uani 1 1 d . . .
H4'A H 0.6960 0.8683 0.1987 0.112 Uiso 1 1 calc R . .
C5' C 0.6592(4) 0.7868(3) 0.23478(15) 0.0953(19) Uani 1 1 d . . .
H5'A H 0.6191 0.7932 0.2428 0.114 Uiso 1 1 calc R . .
C6' C 0.6725(3) 0.7326(3) 0.24840(13) 0.0718(13) Uani 1 1 d . . .
C7' C 0.6247(4) 0.6818(3) 0.27497(14) 0.0882(17) Uani 1 1 d . . .
C8' C 0.6006(5) 0.6381(4) 0.29606(15) 0.115(2) Uani 1 1 d . . .
C9' C 0.5589(4) 0.5808(3) 0.32164(14) 0.0887(18) Uani 1 1 d . . .
C10' C 0.5898(3) 0.5406(3) 0.33361(14) 0.0902(18) Uani 1 1 d . . .
H10B H 0.6361 0.5484 0.3247 0.108 Uiso 1 1 calc R . .
C11' C 0.5544(3) 0.4880(3) 0.35881(13) 0.0843(17) Uani 1 1 d . . .
H11B H 0.5780 0.4613 0.3669 0.101 Uiso 1 1 calc R . .
N12' N 0.4895(2) 0.4738(2) 0.37194(10) 0.0708(11) Uani 1 1 d . . .
C13' C 0.4578(4) 0.5096(5) 0.35908(18) 0.133(3) Uani 1 1 d . . .
H13B H 0.4091 0.4974 0.3669 0.159 Uiso 1 1 calc R . .
C14' C 0.4907(5) 0.5641(5) 0.3349(2) 0.154(4) Uani 1 1 d . . .
H14B H 0.4660 0.5901 0.3273 0.185 Uiso 1 1 calc R . .
B1 B 0.6667 0.3333 0.3333 0.040(5) Uiso 0.48 6 d SPD . .
F1 F 0.6667 0.3333 0.3002(3) 0.047(4) Uiso 0.24 3 d SPD . .
F2 F 0.6327(12) 0.3756(12) 0.3434(4) 0.143(6) Uiso 0.24 1 d PD . .
B10 B 0.6667 0.3333 0.1882(2) 0.065(2) Uiso 1 3 d SD . .
F11 F 0.6667 0.3333 0.22368(15) 0.1103(19) Uiso 1 3 d SD . .
F12 F 0.63239(15) 0.37367(15) 0.17761(6) 0.0668(7) Uiso 1 1 d D . .
B20 B 0.3302(9) 0.4497(8) 0.1858(4) 0.059(5) Uiso 0.25 1 d PD . .
F21 F 0.2942(6) 0.3947(6) 0.1632(2) 0.070(3) Uiso 0.25 1 d PD . .
F22 F 0.2929(15) 0.4904(15) 0.1921(7) 0.290(16) Uiso 0.25 1 d PD . .
F23 F 0.4037(11) 0.5018(13) 0.1769(7) 0.311(18) Uiso 0.25 1 d PD . .
F24 F 0.3334(17) 0.4186(15) 0.2167(5) 0.296(16) Uiso 0.25 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'
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'
Cu Cu 0.3201 1.2651 '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'
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
N12 Cu1 N12' 118.19(15) 2_655 17 y
N12 Cu1 N1 125.82(14) 2_655 . y
N12' Cu1 N1 104.18(15) 17 . y
N12 Cu1 N1' 109.58(15) 2_655 . y
N12' Cu1 N1' 113.23(16) 17 . y
N1 Cu1 N1' 79.80(15) . . y
C6 N1 C2 117.2(4) . . ?
C6 N1 Cu1 127.1(3) . . y
C2 N1 Cu1 115.1(3) . . y
N1 C2 C3 122.1(4) . . ?
N1 C2 C2' 115.5(4) . . ?
C3 C2 C2' 122.4(4) . . ?
C2 C3 C4 119.1(4) . . ?
C5 C4 C3 119.1(5) . . ?
C4 C5 C6 118.4(5) . . ?
N1 C6 C5 124.0(4) . . ?
N1 C6 C7 116.0(4) . . ?
C5 C6 C7 120.0(4) . . ?
C8 C7 C6 173.1(6) . . ?
C7 C8 C9 175.2(6) . . ?
C14 C9 C10 117.8(4) . . ?
C14 C9 C8 120.6(4) . . ?
C10 C9 C8 121.6(4) . . ?
C11 C10 C9 118.5(4) . . ?
N12 C11 C10 124.4(4) . . ?
C11 N12 C13 116.6(4) . . ?
C11 N12 Cu1 123.8(3) . 3_665 y
C13 N12 Cu1 119.6(3) . 3_665 y
N12 C13 C14 124.6(4) . . ?
C13 C14 C9 118.0(4) . . ?
C6' N1' C2' 117.7(4) . . ?
C6' N1' Cu1 128.8(3) . . y
C2' N1' Cu1 112.8(3) . . y
N1' C2' C3' 121.3(4) . . ?
N1' C2' C2 115.7(4) . . ?
C3' C2' C2 123.0(4) . . ?
C4' C3' C2' 119.5(5) . . ?
C3' C4' C5' 119.1(5) . . ?
C6' C5' C4' 119.1(5) . . ?
N1' C6' C5' 123.3(5) . . ?
N1' C6' C7' 114.9(5) . . ?
C5' C6' C7' 121.7(5) . . ?
C8' C7' C6' 163.9(7) . . ?
C7' C8' C9' 171.6(9) . . ?
C10' C9' C14' 116.0(5) . . ?
C10' C9' C8' 118.2(6) . . ?
C14' C9' C8' 125.8(6) . . ?
C9' C10' C11' 120.7(5) . . ?
N12' C11' C10' 122.6(5) . . ?
C13' N12' C11' 116.6(5) . . ?
C13' N12' Cu1 119.5(4) . 18_545 y
C11' N12' Cu1 122.8(3) . 18_545 y
N12' C13' C14' 123.7(7) . . ?
C9' C14' C13' 120.2(6) . . ?
F1 B1 F2 106.6(8) . 2_655 ?
F12 B10 F11 107.7(3) . . ?
F21 B20 F22 112.5(11) . . ?
F21 B20 F23 113.5(11) . . ?
F21 B20 F24 110.2(11) . . ?
F22 B20 F23 107.0(11) . . ?
F22 B20 F24 105.8(10) . . ?
F23 B20 F24 107.4(11) . . ?
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
Cu1 N1 2.060(4) . y
Cu1 N1' 2.113(4) . y
Cu1 N12 1.996(3) 2_655 y
Cu1 N12' 2.041(4) 17 y
N1 C6 1.342(6) . ?
N1 C2 1.356(5) . ?
C2 C3 1.393(6) . ?
C2 C2' 1.486(6) . ?
C3 C4 1.405(7) . ?
C4 C5 1.359(6) . ?
C5 C6 1.401(7) . ?
C6 C7 1.476(6) . ?
C7 C8 1.166(6) . ?
C8 C9 1.439(6) . ?
C9 C14 1.405(6) . ?
C9 C10 1.411(6) . ?
C10 C11 1.365(6) . ?
C11 N12 1.334(5) . ?
N12 C13 1.339(6) . ?
C13 C14 1.371(6) . ?
N1' C6' 1.333(6) . ?
N1' C2' 1.371(5) . ?
C2' C3' 1.415(6) . ?
C3' C4' 1.354(7) . ?
C4' C5' 1.395(7) . ?
C5' C6' 1.382(7) . ?
C6' C7' 1.469(7) . ?
C7' C8' 1.148(7) . ?
C8' C9' 1.468(8) . ?
C9' C10' 1.351(8) . ?
C9' C14' 1.367(9) . ?
C10' C11' 1.388(7) . ?
C11' N12' 1.320(6) . ?
N12' C13' 1.304(7) . ?
C13' C14' 1.375(9) . ?
B1 F1 1.329(11) . ?
B1 F2 1.411(12) . ?
B10 F12 1.390(3) 3_665 ?
B10 F12 1.390(3) 2_655 ?
B10 F12 1.390(3) . ?
B10 F11 1.426(9) . ?
B20 F21 1.345(12) . ?
B20 F23 1.387(13) . ?
B20 F22 1.407(13) . ?
B20 F24 1.410(13) . ?
