#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:34:00 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179796 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/92/7009273.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_7009273
loop_
_publ_author_name
'Paul, Rowena L.'
'Couchman, Samantha M.'
'Jeffery, John C.'
'McCleverty, Jon A.'
'Reeves, Zoe R.'
'Ward, Michael D.'
_publ_section_title
;
 Effects of metal co-ordination geometry on self-assembly: a dinuclear
 double helicate complex and a tetranuclear cage complex of a new
 bis-bidentate bridging ligand
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              845
_journal_paper_doi               10.1039/a909702c
_journal_year                    2000
_chemical_formula_sum            'C32 H27 B Cu F4 N6 O2'
_chemical_formula_weight         677.95
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.561(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.702(3)
_cell_length_b                   20.284(4)
_cell_length_c                   20.669(6)
_cell_measurement_temperature    173(2)
_cell_volume                     6144(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method
'ω rotation with narrow frames (0.3 degrees)'
_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  0.0801
_diffrn_reflns_av_sigmaI/netI    0.1131
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19097
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.954
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_restrained_S_obs      1.112
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_obs          0.0654
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0848P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1773
_refine_ls_wR_factor_obs         0.1442
_reflns_number_observed          3547
_reflns_number_total             6969
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a909702c.txt
_cod_data_source_block           /tintin3/people/sam/wish/wishes
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6144.1(25)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009273
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu1 Cu 1.19575(3) 1.41643(3) 0.52198(3) 0.0336(2) Uani 1 d . .
C1 C 1.1250(5) 1.2653(3) 0.3972(4) 0.099(3) Uani 1 d . .
H1A H 1.1447(5) 1.2291(3) 0.4264(4) 0.148 Uiso 1 calc R .
H1B H 1.1545(5) 1.2610(3) 0.3565(4) 0.148 Uiso 1 calc R .
H1C H 1.0587(5) 1.2636(3) 0.3881(4) 0.148 Uiso 1 calc R .
O1 O 1.1323(2) 1.3792(2) 0.3994(2) 0.0633(11) Uani 1 d . .
O2 O 1.1879(2) 1.3280(2) 0.4869(2) 0.0499(9) Uani 1 d . .
C2 C 1.1523(3) 1.3320(3) 0.4298(2) 0.0380(12) Uani 1 d . .
N111 N 1.1839(2) 1.5127(2) 0.5475(2) 0.0324(9) Uani 1 d . .
C112 C 1.1044(3) 1.5282(2) 0.5721(2) 0.0308(10) Uani 1 d . .
C113 C 1.0863(3) 1.5913(2) 0.5937(2) 0.0388(11) Uani 1 d . .
H11A H 1.0299(3) 1.6009(2) 0.6111(2) 0.047 Uiso 1 calc R .
C114 C 1.1511(4) 1.6397(3) 0.5895(3) 0.0472(13) Uani 1 d . .
H11B H 1.1403(4) 1.6830(3) 0.6046(3) 0.057 Uiso 1 calc R .
C115 C 1.2319(3) 1.6249(3) 0.5632(3) 0.0507(14) Uani 1 d . .
H11C H 1.2770(3) 1.6579(3) 0.5591(3) 0.061 Uiso 1 calc R .
C116 C 1.2458(3) 1.5610(2) 0.5427(2) 0.0422(12) Uani 1 d . .
H11D H 1.3014(3) 1.5508(2) 0.5245(2) 0.051 Uiso 1 calc R .
N121 N 1.0689(2) 1.4141(2) 0.5556(2) 0.0303(8) Uani 1 d . .
C122 C 1.0399(3) 1.4734(2) 0.5744(2) 0.0305(10) Uani 1 d . .
C123 C 0.9506(3) 1.4701(2) 0.5909(2) 0.0337(11) Uani 1 d . .
H12A H 0.9146(3) 1.5051(2) 0.6055(2) 0.040 Uiso 1 calc R .
C124 C 0.9256(3) 1.4060(2) 0.5816(2) 0.0377(12) Uani 1 d . .
H12B H 0.8677(3) 1.3879(2) 0.5888(2) 0.045 Uiso 1 calc R .
N125 N 0.9968(2) 1.3724(2) 0.5605(2) 0.0326(9) Uani 1 d . .
C126 C 1.0007(3) 1.3013(2) 0.5486(2) 0.0367(11) Uani 1 d . .
H12C H 1.0389(3) 1.2928(2) 0.5121(2) 0.044 Uiso 1 calc R .
H12D H 0.9385(3) 1.2848(2) 0.5360(2) 0.044 Uiso 1 calc R .
C131 C 1.0402(3) 1.2644(2) 0.6087(2) 0.0347(11) Uani 1 d . .
C132 C 1.1256(3) 1.2359(2) 0.6106(2) 0.0405(12) Uani 1 d . .
H13A H 1.1590(3) 1.2369(2) 0.5732(2) 0.049 Uiso 1 calc R .
C133 C 1.1628(3) 1.2059(2) 0.6669(3) 0.0473(13) Uani 1 d . .
H13B H 1.2215(3) 1.1862(2) 0.6677(3) 0.057 Uiso 1 calc R .
C134 C 1.1139(3) 1.2044(2) 0.7228(2) 0.0409(12) Uani 1 d . .
H13C H 1.1404(3) 1.1851(2) 0.7617(2) 0.049 Uiso 1 calc R .
C135 C 1.0265(3) 1.2314(2) 0.7210(2) 0.0335(10) Uani 1 d . .
C136 C 0.9897(3) 1.2604(2) 0.6638(2) 0.0346(11) Uani 1 d . .
H13D H 0.9295(3) 1.2779(2) 0.6619(2) 0.041 Uiso 1 calc R .
N211 N 1.3180(2) 1.4307(2) 0.4821(2) 0.0393(10) Uani 1 d . .
C212 C 1.3954(3) 1.4147(2) 0.5178(2) 0.0403(11) Uani 1 d . .
C213 C 1.4796(3) 1.4134(3) 0.4918(3) 0.0523(14) Uani 1 d . .
H21A H 1.5333(3) 1.4013(3) 0.5177(3) 0.063 Uiso 1 calc R .
C214 C 1.4834(3) 1.4301(3) 0.4274(3) 0.0554(15) Uani 1 d . .
H21B H 1.5399(3) 1.4284(3) 0.4082(3) 0.067 Uiso 1 calc R .
C215 C 1.4063(3) 1.4491(3) 0.3914(3) 0.0514(14) Uani 1 d . .
H21C H 1.4090(3) 1.4630(3) 0.3477(3) 0.062 Uiso 1 calc R .
C216 C 1.3236(3) 1.4478(2) 0.4196(2) 0.0414(12) Uani 1 d . .
H21D H 1.2694(3) 1.4593(2) 0.3941(2) 0.050 Uiso 1 calc R .
N221 N 1.2991(2) 1.3948(2) 0.6053(2) 0.0393(10) Uani 1 d . .
C222 C 1.3842(3) 1.4011(3) 0.5868(3) 0.0463(13) Uani 1 d . .
C223 C 1.4488(4) 1.3915(3) 0.6392(3) 0.064(2) Uani 1 d . .
H22A H 1.5134(4) 1.3934(3) 0.6388(3) 0.077 Uiso 1 calc R .
C224 C 1.3992(3) 1.3787(3) 0.6911(3) 0.064(2) Uani 1 d . .
H22B H 1.4231(3) 1.3703(3) 0.7344(3) 0.077 Uiso 1 calc R .
N225 N 1.3096(3) 1.3802(2) 0.6692(2) 0.0478(11) Uani 1 d . .
C226 C 1.2306(3) 1.3725(3) 0.7069(2) 0.0446(13) Uani 1 d . .
H22C H 1.2495(3) 1.3490(3) 0.7478(2) 0.053 Uiso 1 calc R .
H22D H 1.1844(3) 1.3450(3) 0.6821(2) 0.053 Uiso 1 calc R .
C231 C 1.1879(3) 1.4377(2) 0.7230(2) 0.0381(11) Uani 1 d . .
C232 C 1.2382(3) 1.4953(3) 0.7338(2) 0.0508(14) Uani 1 d . .
H23A H 1.3021(3) 1.4952(3) 0.7297(2) 0.061 Uiso 1 calc R .
C233 C 1.1946(4) 1.5527(3) 0.7504(3) 0.0550(15) Uani 1 d . .
H23B H 1.2289(4) 1.5922(3) 0.7569(3) 0.066 Uiso 1 calc R .
C234 C 1.1027(4) 1.5532(3) 0.7576(2) 0.0479(13) Uani 1 d . .
H23C H 1.0748(4) 1.5929(3) 0.7703(2) 0.058 Uiso 1 calc R .
C235 C 1.0493(3) 1.4971(2) 0.7467(2) 0.0381(11) Uani 1 d . .
C236 C 1.0945(3) 1.4392(2) 0.7287(2) 0.0355(11) Uani 1 d . .
H23D H 1.0599(3) 1.4001(2) 0.7201(2) 0.043 Uiso 1 calc R .
B1 B 1.1837(4) 1.8240(3) 0.6072(3) 0.0471(15) Uani 1 d . .
F11 F 1.1905(3) 1.8910(2) 0.6068(2) 0.0958(13) Uani 1 d . .
F12 F 1.1449(2) 1.8035(2) 0.6632(2) 0.0832(11) Uani 1 d . .
F13 F 1.1284(2) 1.8032(2) 0.5553(2) 0.0764(10) Uani 1 d . .
F14 F 1.2690(2) 1.7951(2) 0.6070(2) 0.0775(11) Uani 1 d . .
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
O2 Cu1 N111 169.57(14) . . ?
O2 Cu1 N121 94.42(14) . . ?
N111 Cu1 N121 80.47(14) . . ?
O2 Cu1 N211 90.47(15) . . ?
N111 Cu1 N211 93.72(15) . . ?
N121 Cu1 N211 172.18(15) . . ?
O2 Cu1 N221 97.06(15) . . ?
N111 Cu1 N221 93.20(14) . . ?
N121 Cu1 N221 108.37(14) . . ?
N211 Cu1 N221 76.99(14) . . ?
C2 O2 Cu1 107.5(3) . . ?
O1 C2 O2 128.8(5) . . ?
O1 C2 C1 115.8(6) . . ?
O2 C2 C1 115.2(5) . . ?
C116 N111 C112 118.0(4) . . ?
C116 N111 Cu1 127.4(3) . . ?
C112 N111 Cu1 114.7(3) . . ?
N111 C112 C113 122.1(4) . . ?
N111 C112 C122 114.6(4) . . ?
C113 C112 C122 123.3(4) . . ?
C114 C113 C112 119.1(5) . . ?
C113 C114 C115 119.5(5) . . ?
C114 C115 C116 118.6(5) . . ?
N111 C116 C115 122.8(5) . . ?
C122 N121 N125 105.5(3) . . ?
C122 N121 Cu1 113.4(3) . . ?
N125 N121 Cu1 140.8(3) . . ?
N121 C122 C123 111.0(4) . . ?
N121 C122 C112 116.7(4) . . ?
C123 C122 C112 132.3(4) . . ?
C124 C123 C122 105.2(4) . . ?
N125 C124 C123 108.7(4) . . ?
C124 N125 N121 109.7(4) . . ?
C124 N125 C126 126.4(4) . . ?
N121 N125 C126 123.8(4) . . ?
N125 C126 C131 111.4(4) . . ?
C132 C131 C136 119.3(4) . . ?
C132 C131 C126 121.0(4) . . ?
C136 C131 C126 119.6(4) . . ?
C131 C132 C133 120.4(4) . . ?
C132 C133 C134 120.2(4) . . ?
C135 C134 C133 119.9(5) . . ?
C136 C135 C134 119.0(4) . . ?
C136 C135 C135 119.5(5) . 2_756 ?
C134 C135 C135 121.4(5) . 2_756 ?
C135 C136 C131 121.0(4) . . ?
C212 N211 C216 118.3(4) . . ?
C212 N211 Cu1 118.3(3) . . ?
C216 N211 Cu1 122.9(3) . . ?
N211 C212 C213 122.3(4) . . ?
N211 C212 C222 114.9(4) . . ?
C213 C212 C222 122.8(4) . . ?
C214 C213 C212 118.3(5) . . ?
C215 C214 C213 120.2(5) . . ?
C214 C215 C216 118.8(5) . . ?
N211 C216 C215 122.0(5) . . ?
C222 N221 N225 105.2(4) . . ?
C222 N221 Cu1 110.6(3) . . ?
N225 N221 Cu1 144.1(3) . . ?
N221 C222 C223 111.0(5) . . ?
N221 C222 C212 118.1(4) . . ?
C223 C222 C212 130.9(4) . . ?
C224 C223 C222 105.2(5) . . ?
N225 C224 C223 107.3(5) . . ?
N221 N225 C224 111.3(4) . . ?
N221 N225 C226 120.8(4) . . ?
C224 N225 C226 127.8(4) . . ?
N225 C226 C231 112.8(4) . . ?
C236 C231 C232 119.0(5) . . ?
C236 C231 C226 118.0(4) . . ?
C232 C231 C226 122.9(4) . . ?
C233 C232 C231 119.7(5) . . ?
C234 C233 C232 120.8(5) . . ?
C233 C234 C235 121.6(5) . . ?
C234 C235 C236 116.9(4) . . ?
C234 C235 C235 122.3(3) . 2_756 ?
C236 C235 C235 120.9(3) . 2_756 ?
C231 C236 C235 121.9(4) . . ?
F13 B1 F11 110.1(5) . . ?
F13 B1 F14 110.6(5) . . ?
F11 B1 F14 110.8(5) . . ?
F13 B1 F12 107.7(5) . . ?
F11 B1 F12 109.8(5) . . ?
F14 B1 F12 107.8(5) . . ?
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 O2 1.934(4) . ?
Cu1 N111 2.033(4) . ?
Cu1 N121 2.042(3) . ?
Cu1 N211 2.056(4) . ?
Cu1 N221 2.247(4) . ?
C1 C2 1.551(8) . ?
O1 C2 1.169(6) . ?
O2 C2 1.255(6) . ?
N111 C116 1.347(6) . ?
N111 C112 1.348(5) . ?
C112 C113 1.387(6) . ?
C112 C122 1.465(6) . ?
C113 C114 1.377(7) . ?
C114 C115 1.378(7) . ?
C115 C116 1.385(7) . ?
N121 C122 1.343(5) . ?
N121 N125 1.366(5) . ?
C122 C123 1.384(6) . ?
C123 C124 1.361(6) . ?
C124 N125 1.351(5) . ?
N125 C126 1.464(6) . ?
C126 C131 1.527(6) . ?
C131 C132 1.379(6) . ?
C131 C136 1.411(6) . ?
C132 C133 1.386(7) . ?
C133 C134 1.411(6) . ?
C134 C135 1.393(6) . ?
C135 C136 1.391(6) . ?
C135 C135 1.482(8) 2_756 ?
N211 C212 1.345(6) . ?
N211 C216 1.346(6) . ?
C212 C213 1.389(6) . ?
C212 C222 1.474(7) . ?
C213 C214 1.378(7) . ?
C214 C215 1.361(7) . ?
C215 C216 1.390(6) . ?
N221 C222 1.343(6) . ?
N221 N225 1.352(5) . ?
C222 C223 1.396(7) . ?
C223 C224 1.370(8) . ?
C224 N225 1.359(6) . ?
N225 C226 1.457(6) . ?
C226 C231 1.512(7) . ?
C231 C236 1.387(6) . ?
C231 C232 1.391(7) . ?
C232 C233 1.386(7) . ?
C233 C234 1.372(7) . ?
C234 C235 1.391(6) . ?
C235 C236 1.414(6) . ?
C235 C235 1.467(9) 2_756 ?
B1 F13 1.360(7) . ?
B1 F11 1.364(7) . ?
B1 F14 1.384(7) . ?
B1 F12 1.393(7) . ?
