#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:30:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180224 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/10/7111021.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111021
loop_
_publ_author_name
'Rice, Craig R.'
'Wörl, Stefan'
'Jeffery, John C.'
'Paul, Rowena L.'
'Ward, Michael D.'
_publ_section_title
;
 Pyridyl-thiazoles as a new class of ligand for metallosupramolecular
 chemistry: formation of double and triple helicates with Cu(ii)
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1529
_journal_paper_doi               10.1039/b004319m
_journal_year                    2000
_chemical_formula_sum            'C30 H27 Cu F12 N6 O2 P2 S3'
_chemical_formula_weight         953.24
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.792(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.9497(14)
_cell_length_b                   23.133(2)
_cell_length_c                   22.485(2)
_cell_measurement_temperature    293(2)
_cell_volume                     7150.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1004
_diffrn_reflns_av_sigmaI/netI    0.1146
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19016
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6291
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1655
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1619P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2332
_refine_ls_wR_factor_ref         0.2807
_reflns_number_gt                3197
_reflns_number_total             6291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004319msup1.cif
_cod_data_source_block           jiffy1m
_cod_original_cell_volume        7150.3(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7111021
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.66657(8) 0.63095(4) 0.76312(5) 0.0347(3) Uani 1 1 d .
N11 N 0.5959(6) 0.5587(3) 0.8011(3) 0.0441(19) Uani 1 1 d .
C12 C 0.5313(7) 0.5485(4) 0.8409(4) 0.046(2) Uani 1 1 d .
C13 C 0.5217(8) 0.4929(5) 0.8541(6) 0.069(3) Uani 1 1 d .
H13 H 0.4789 0.4791 0.8783 0.083 Uiso 1 1 calc R
S14 S 0.5978(2) 0.45032(12) 0.82098(17) 0.0718(10) Uani 1 1 d .
C15 C 0.6361(7) 0.5099(4) 0.7873(4) 0.047(2) Uani 1 1 d .
N21 N 0.7427(6) 0.5633(4) 0.7375(3) 0.048(2) Uani 1 1 d .
C22 C 0.7148(7) 0.5100(4) 0.7511(4) 0.049(2) Uani 1 1 d .
C23 C 0.7575(9) 0.4607(5) 0.7344(5) 0.066(3) Uani 1 1 d .
H23 H 0.7345 0.4246 0.7436 0.079 Uiso 1 1 calc R
C24 C 0.8358(9) 0.4652(6) 0.7035(5) 0.073(4) Uani 1 1 d .
H24 H 0.8673 0.4324 0.6926 0.087 Uiso 1 1 calc R
C25 C 0.8649(11) 0.5195(7) 0.6899(6) 0.097(5) Uani 1 1 d .
H25 H 0.9163 0.5240 0.6688 0.116 Uiso 1 1 calc R
C26 C 0.8172(9) 0.5679(5) 0.7077(5) 0.065(3) Uani 1 1 d .
H26 H 0.8380 0.6045 0.6984 0.078 Uiso 1 1 calc R
N31 N 0.5982(5) 0.6962(3) 0.8019(3) 0.0385(17) Uani 1 1 d .
C32 C 0.6381(7) 0.7074(4) 0.8576(4) 0.042(2) Uani 1 1 d .
S33 S 0.5931(2) 0.76651(11) 0.88828(12) 0.0540(7) Uani 1 1 d .
C34 C 0.5144(7) 0.7778(4) 0.8214(5) 0.051(3) Uani 1 1 d .
H34 H 0.4698 0.8080 0.8140 0.061 Uiso 1 1 calc R
C35 C 0.5277(7) 0.7362(4) 0.7813(4) 0.041(2) Uani 1 1 d .
N41 N 0.7575(6) 0.6359(3) 0.8526(4) 0.051(2) Uani 1 1 d .
C42 C 0.7183(7) 0.6701(4) 0.8892(4) 0.049(2) Uani 1 1 d .
C43 C 0.7452(9) 0.6718(5) 0.9515(5) 0.065(3) Uani 1 1 d .
H43 H 0.7166 0.6977 0.9749 0.078 Uiso 1 1 calc R
C44 C 0.8171(11) 0.6332(5) 0.9777(6) 0.088(4) Uani 1 1 d .
H44 H 0.8330 0.6296 1.0194 0.106 Uiso 1 1 calc R
C45 C 0.8651(11) 0.5998(5) 0.9391(6) 0.087(5) Uani 1 1 d .
H45 H 0.9182 0.5770 0.9547 0.104 Uiso 1 1 calc R
C46 C 0.8316(8) 0.6018(5) 0.8779(6) 0.067(3) Uani 1 1 d .
H46 H 0.8615 0.5785 0.8528 0.081 Uiso 1 1 calc R
N51 N 0.4151(6) 0.6315(3) 0.8306(3) 0.0430(18) Uani 1 1 d .
C52 C 0.3765(7) 0.6675(4) 0.8648(4) 0.041(2) Uani 1 1 d .
S53 S 0.4181(2) 0.66249(12) 0.94030(12) 0.0595(8) Uani 1 1 d .
C54 C 0.4945(8) 0.6083(4) 0.9263(5) 0.057(3) Uani 1 1 d .
H54 H 0.5380 0.5893 0.9558 0.069 Uiso 1 1 calc R
C55 C 0.4831(7) 0.5969(4) 0.8666(5) 0.049(2) Uani 1 1 d .
N61 N 0.2610(6) 0.6980(3) 0.7803(3) 0.047(2) Uani 1 1 d .
C62 C 0.2994(7) 0.7085(4) 0.8375(4) 0.042(2) Uani 1 1 d .
C63 C 0.2703(8) 0.7550(4) 0.8692(5) 0.052(3) Uani 1 1 d .
H63 H 0.3001 0.7618 0.9088 0.062 Uiso 1 1 calc R
C64 C 0.1987(9) 0.7906(5) 0.8424(5) 0.065(3) Uani 1 1 d .
H64 H 0.1776 0.8215 0.8633 0.078 Uiso 1 1 calc R
C65 C 0.1575(8) 0.7795(5) 0.7822(6) 0.068(3) Uani 1 1 d .
H65 H 0.1071 0.8023 0.7623 0.082 Uiso 1 1 calc R
C66 C 0.1937(9) 0.7340(5) 0.7533(5) 0.064(3) Uani 1 1 d .
H66 H 0.1694 0.7282 0.7125 0.076 Uiso 1 1 calc R
C71 C 0.6810(16) 0.4875(8) 0.0391(10) 0.118(6) Uani 1 1 d U
C72 C 0.6077(18) 0.4978(8) 0.0048(9) 0.146(7) Uani 1 1 d U
O73 O 0.6775(12) 0.4798(8) 0.0946(7) 0.181(7) Uani 1 1 d U
C74 C 0.767(2) 0.4831(14) 0.0169(15) 0.235(14) Uani 1 1 d U
C81 C 0.399(3) 0.8549(18) 0.0971(18) 0.257(16) Uani 1 1 d U
C82 C 0.334(3) 0.864(2) 0.073(3) 0.31(2) Uani 1 1 d U
O83 O 0.4367(17) 0.7981(8) 0.0469(7) 0.221(8) Uani 1 1 d U
C84 C 0.304(2) 0.8248(9) 0.0206(11) 0.187(10) Uani 1 1 d U
P1 P 0.6005(3) 0.66158(14) 0.10842(15) 0.0717(10) Uani 1 1 d .
F11 F 0.4917(7) 0.6446(4) 0.0786(4) 0.131(4) Uani 1 1 d .
F12 F 0.5562(6) 0.7145(4) 0.1393(3) 0.099(2) Uani 1 1 d .
F13 F 0.5920(7) 0.6233(3) 0.1657(4) 0.114(3) Uani 1 1 d .
F14 F 0.7016(6) 0.6802(5) 0.1431(5) 0.147(4) Uani 1 1 d .
F15 F 0.6407(12) 0.6102(5) 0.0780(5) 0.189(6) Uani 1 1 d .
F16 F 0.6038(8) 0.7000(4) 0.0502(4) 0.130(3) Uani 1 1 d .
P2 P 0.4325(2) 0.92245(11) 0.89368(13) 0.0518(7) Uani 1 1 d .
F21 F 0.3245(6) 0.9347(6) 0.8862(4) 0.159(5) Uani 1 1 d .
F22 F 0.4442(6) 0.9430(4) 0.9612(3) 0.109(3) Uani 1 1 d .
F23 F 0.4353(9) 0.8585(3) 0.9153(4) 0.134(4) Uani 1 1 d .
F24 F 0.5454(6) 0.9121(5) 0.8988(4) 0.139(4) Uani 1 1 d .
F25 F 0.4423(9) 0.9842(3) 0.8679(6) 0.154(4) Uani 1 1 d .
F26 F 0.4194(9) 0.8997(4) 0.8276(3) 0.154(5) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
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'
S S 0.1246 0.1234 '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'
P P 0.1023 0.0942 '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'
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
N21 Cu1 N31 171.5(3) . .
N21 Cu1 N61 96.7(3) . 2_656
N31 Cu1 N61 87.2(3) . 2_656
N21 Cu1 N11 79.2(3) . .
N31 Cu1 N11 97.1(3) . .
N61 Cu1 N11 175.4(3) 2_656 .
N21 Cu1 N41 92.9(3) . .
N31 Cu1 N41 79.1(3) . .
N61 Cu1 N41 97.8(3) 2_656 .
N11 Cu1 N41 84.8(3) . .
N21 Cu1 N51 86.8(3) . 2_656
N31 Cu1 N51 101.4(3) . 2_656
N61 Cu1 N51 76.8(3) 2_656 2_656
N11 Cu1 N51 100.5(3) . 2_656
N41 Cu1 N51 174.5(3) . 2_656
C15 N11 C12 110.7(8) . .
C15 N11 Cu1 108.9(6) . .
C12 N11 Cu1 139.8(6) . .
C13 C12 N11 114.1(9) . .
C13 C12 C55 125.1(10) . .
N11 C12 C55 120.8(8) . .
C12 C13 S14 111.4(9) . .
C15 S14 C13 89.6(5) . .
N11 C15 C22 121.0(9) . .
N11 C15 S14 114.1(8) . .
C22 C15 S14 124.5(7) . .
C26 N21 C22 117.9(9) . .
C26 N21 Cu1 124.9(7) . .
C22 N21 Cu1 117.3(6) . .
N21 C22 C23 123.1(10) . .
N21 C22 C15 113.5(8) . .
C23 C22 C15 123.4(10) . .
C22 C23 C24 119.3(12) . .
C25 C24 C23 117.8(11) . .
C24 C25 C26 119.8(12) . .
N21 C26 C25 122.1(12) . .
C32 N31 C35 110.6(7) . .
C32 N31 Cu1 113.6(6) . .
C35 N31 Cu1 135.2(6) . .
N31 C32 C42 120.2(8) . .
N31 C32 S33 115.0(7) . .
C42 C32 S33 124.8(7) . .
C32 S33 C34 89.6(5) . .
C35 C34 S33 109.5(7) . .
C34 C35 N31 115.3(8) . .
C34 C35 C35 121.5(8) . 2_656
N31 C35 C35 123.1(7) . 2_656
C42 N41 C46 117.2(9) . .
C42 N41 Cu1 111.5(6) . .
C46 N41 Cu1 129.7(7) . .
N41 C42 C43 125.1(10) . .
N41 C42 C32 113.8(8) . .
C43 C42 C32 121.0(10) . .
C42 C43 C44 117.2(11) . .
C43 C44 C45 118.2(12) . .
C46 C45 C44 118.7(11) . .
N41 C46 C45 123.1(11) . .
C52 N51 C55 109.4(8) . .
C52 N51 Cu1 111.4(6) . 2_656
C55 N51 Cu1 137.6(6) . 2_656
N51 C52 C62 120.3(8) . .
N51 C52 S53 115.9(7) . .
C62 C52 S53 123.8(7) . .
C52 S53 C54 89.1(5) . .
C55 C54 S53 110.8(8) . .
C54 C55 N51 114.8(8) . .
C54 C55 C12 123.7(10) . .
N51 C55 C12 121.4(9) . .
C66 N61 C62 117.9(9) . .
C66 N61 Cu1 126.2(7) . 2_656
C62 N61 Cu1 115.1(6) . 2_656
N61 C62 C63 122.2(9) . .
N61 C62 C52 115.3(8) . .
C63 C62 C52 122.5(8) . .
C64 C63 C62 120.1(10) . .
C63 C64 C65 117.9(11) . .
C66 C65 C64 118.3(11) . .
N61 C66 C65 123.5(10) . .
C72 C71 O73 119(2) . .
C72 C71 C74 119(3) . .
O73 C71 C74 122(2) . .
C82 C81 O83 98(5) . .
C81 C82 C84 114(6) . .
F15 P1 F14 94.0(7) . .
F15 P1 F12 178.6(7) . .
F14 P1 F12 87.4(5) . .
F15 P1 F13 90.7(6) . .
F14 P1 F13 86.2(6) . .
F12 P1 F13 89.3(5) . .
F15 P1 F16 90.2(6) . .
F14 P1 F16 96.2(6) . .
F12 P1 F16 89.8(5) . .
F13 P1 F16 177.4(6) . .
F15 P1 F11 90.9(7) . .
F14 P1 F11 174.0(6) . .
F12 P1 F11 87.7(5) . .
F13 P1 F11 90.4(5) . .
F16 P1 F11 87.2(5) . .
F21 P2 F23 100.6(7) . .
F21 P2 F25 86.3(7) . .
F23 P2 F25 171.9(6) . .
F21 P2 F26 90.3(6) . .
F23 P2 F26 88.3(5) . .
F25 P2 F26 87.6(6) . .
F21 P2 F22 89.3(5) . .
F23 P2 F22 89.6(5) . .
F25 P2 F22 94.7(6) . .
F26 P2 F22 177.7(6) . .
F21 P2 F24 177.0(6) . .
F23 P2 F24 82.0(6) . .
F25 P2 F24 90.9(6) . .
F26 P2 F24 88.4(6) . .
F22 P2 F24 92.2(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N21 2.028(8) .
Cu1 N31 2.056(7) .
Cu1 N61 2.171(8) 2_656
Cu1 N11 2.187(8) .
Cu1 N41 2.192(8) .
Cu1 N51 2.219(8) 2_656
N11 C15 1.321(11) .
N11 C12 1.393(12) .
C12 C13 1.331(14) .
C12 C55 1.474(12) .
C13 S14 1.710(11) .
S14 C15 1.703(10) .
C15 C22 1.473(14) .
N21 C26 1.334(13) .
N21 C22 1.344(13) .
C22 C23 1.367(13) .
C23 C24 1.395(16) .
C24 C25 1.371(19) .
C25 C26 1.396(16) .
N31 C32 1.308(11) .
N31 C35 1.373(11) .
C32 C42 1.494(13) .
C32 S33 1.699(9) .
S33 C34 1.724(11) .
C34 C35 1.353(12) .
C35 C35 1.486(18) 2_656
N41 C42 1.325(12) .
N41 C46 1.346(12) .
C42 C43 1.388(14) .
C43 C44 1.396(16) .
C44 C45 1.411(18) .
C45 C46 1.378(16) .
N51 C52 1.311(11) .
N51 C55 1.390(12) .
N51 Cu1 2.219(8) 2_656
C52 C62 1.485(13) .
C52 S53 1.702(9) .
S53 C54 1.709(10) .
C54 C55 1.350(14) .
N61 C66 1.324(13) .
N61 C62 1.329(11) .
N61 Cu1 2.171(8) 2_656
C62 C63 1.390(12) .
C63 C64 1.354(14) .
C64 C65 1.402(16) .
C65 C66 1.377(15) .
C71 C72 1.19(2) .
C71 O73 1.27(2) .
C71 C74 1.37(3) .
C81 C82 1.00(8) .
C81 O83 1.86(4) .
C82 C84 1.49(5) .
P1 F15 1.525(10) .
P1 F14 1.552(10) .
P1 F12 1.582(8) .
P1 F13 1.585(8) .
P1 F16 1.590(8) .
P1 F11 1.600(9) .
P2 F21 1.515(8) .
P2 F23 1.556(8) .
P2 F25 1.557(8) .
P2 F26 1.558(8) .
P2 F22 1.573(8) .
P2 F24 1.577(8) .
