#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:36:43 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180189 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/85/7108551.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_7108551
loop_
_publ_author_name
'Samir Barman'
'Jai Anand Garg'
'Olivier Blacque'
'Koushik Venkatesan'
'Heinz Berke'
_publ_section_title
;
 Triptycene based luminescent metal-organic gels for chemosensing
;
_journal_name_full               Chem.Commun.
_journal_page_first              11127
_journal_paper_doi               10.1039/c2cc34430k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C27 H19 Co2 N O10'
_chemical_formula_sum            'C27 H19 Co2 N O10'
_chemical_formula_weight         635.29
_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                 98.302(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1691(5)
_cell_length_b                   11.0334(5)
_cell_length_c                   16.3274(6)
_cell_measurement_reflns_used    3441
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.75
_cell_measurement_theta_min      2.44
_cell_volume                     3060.5(2)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.33.55 (Agilent, 2011)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.33.55 (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.33.55 (Agilent, 2011)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 1999), PLATON for Windows (Spek, 2003) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement  ' SHELXL97. Sheldrick (2008).'
_computing_structure_solution    ' SHELXS97. Sheldrick (2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9118
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.33.66 (Agilent, 2011)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by Clark & Reid (1995).
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2691
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1219P)²+11.3813P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2256
_reflns_number_gt                1970
_reflns_number_total             2691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34430k.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7108551
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0957(4) 0.3200(6) 0.1340(4) 0.0368(15) Uani 1 1 d . . .
C2 C 0.1693(4) 0.2485(7) 0.1290(4) 0.0391(16) Uani 1 1 d . . .
C5 C 0.3080(4) 0.1107(6) 0.1282(4) 0.0368(16) Uani 1 1 d . . .
C3A C 0.1842(9) 0.1489(17) 0.1777(11) 0.046(4) Uani 0.50 1 d P . .
H3A H 0.1483 0.1268 0.2126 0.056 Uiso 0.50 1 calc PR . .
C4A C 0.2528(11) 0.0776(18) 0.1770(12) 0.057(5) Uani 0.50 1 d P . .
H4A H 0.2604 0.0083 0.2096 0.069 Uiso 0.50 1 calc PR . .
C6A C 0.2968(6) 0.2161(12) 0.0806(8) 0.032(3) Uani 0.50 1 d P . .
C7A C 0.2285(7) 0.2884(11) 0.0816(7) 0.030(3) Uani 0.50 1 d P . .
C3B C 0.2138(9) 0.212(2) 0.2026(10) 0.053(5) Uani 0.50 1 d P . .
H3B H 0.1970 0.2317 0.2526 0.064 Uiso 0.50 1 calc PR . .
C4B C 0.2834(10) 0.1476(17) 0.2026(10) 0.050(4) Uani 0.50 1 d P . .
H4B H 0.3140 0.1286 0.2527 0.060 Uiso 0.50 1 calc PR . .
C6B C 0.2589(7) 0.1353(11) 0.0545(8) 0.031(3) Uani 0.50 1 d P . .
C7B C 0.1901(7) 0.2046(12) 0.0544(8) 0.030(3) Uani 0.50 1 d P . .
C8 C 0.3845(4) 0.0378(6) 0.1339(4) 0.0380(16) Uani 1 1 d . . .
C9 C 0.3553(7) 0.2764(11) 0.0296(7) 0.029(3) Uani 0.50 1 d P . .
H9 H 0.4034 0.2288 0.0288 0.035 Uiso 0.50 1 calc PR . .
C10 C 0.2275(7) 0.4018(12) 0.0320(8) 0.034(3) Uani 0.50 1 d P . .
H10 H 0.1795 0.4496 0.0324 0.041 Uiso 0.50 1 calc PR . .
C11 C 0.3034(4) 0.4723(7) 0.0659(6) 0.039(3) Uani 0.50 1 d PG . .
C12 C 0.3714(5) 0.4042(6) 0.0652(6) 0.032(3) Uani 0.50 1 d PG . .
C13 C 0.4446(4) 0.4555(8) 0.0919(6) 0.052(4) Uani 0.50 1 d PG . .
H13 H 0.4901 0.4099 0.0914 0.062 Uiso 0.50 1 calc PR . .
C14 C 0.4498(4) 0.5749(9) 0.1192(7) 0.074(6) Uani 0.50 1 d PG . .
H14 H 0.4988 0.6092 0.1370 0.089 Uiso 0.50 1 calc PR . .
C15 C 0.3818(6) 0.6430(6) 0.1199(7) 0.056(4) Uani 0.50 1 d PG . .
H15 H 0.3853 0.7229 0.1382 0.067 Uiso 0.50 1 calc PR . .
C16 C 0.3086(5) 0.5917(7) 0.0933(6) 0.047(4) Uani 0.50 1 d PG . .
H16 H 0.2631 0.6373 0.0937 0.056 Uiso 0.50 1 calc PR . .
O1 O 0.0609(3) 0.2966(5) 0.1939(3) 0.0534(14) Uani 1 1 d . . .
O2 O 0.0753(3) 0.3981(6) 0.0835(4) 0.080(2) Uani 1 1 d . A .
O3 O 0.4082(3) 0.0041(6) 0.0703(4) 0.078(2) Uani 1 1 d . . .
O4 O 0.4153(4) 0.0150(6) 0.2044(3) 0.080(2) Uani 1 1 d . . .
O5 O -0.0505(10) 0.3547(16) -0.0716(9) 0.079(5) Uani 0.50 1 d PD A -1
O6 O 0.054(2) 0.659(2) 0.0349(12) 0.138(5) Uani 0.50 1 d PD A -2
N1 N 0.1091(13) 0.7923(16) 0.1337(10) 0.138(5) Uani 0.50 1 d PD A -2
C17 C 0.0739(19) 0.699(2) 0.1021(12) 0.138(5) Uani 0.50 1 d PD A -2
H17 H 0.0600 0.6471 0.1427 0.165 Uiso 0.50 1 calc PR A -2
C18 C 0.1532(16) 0.852(2) 0.0922(14) 0.138(5) Uani 0.50 1 d PD A -2
H18A H 0.1671 0.8017 0.0483 0.206 Uiso 0.50 1 calc PR A -2
H18B H 0.2001 0.8758 0.1277 0.206 Uiso 0.50 1 calc PR A -2
H18C H 0.1258 0.9224 0.0690 0.206 Uiso 0.50 1 calc PR A -2
C19 C 0.1128(18) 0.812(2) 0.2108(13) 0.138(5) Uani 0.50 1 d PD A -2
H19A H 0.0968 0.8938 0.2195 0.206 Uiso 0.50 1 calc PR A -2
H19B H 0.1658 0.8001 0.2374 0.206 Uiso 0.50 1 calc PR A -2
H19C H 0.0785 0.7568 0.2337 0.206 Uiso 0.50 1 calc PR A -2
Co1 Co 0.0000 0.40958(12) 0.2500 0.0328(4) Uani 1 2 d S . .
Co2 Co 0.0000 0.5000 0.0000 0.0406(4) Uani 1 2 d SD . .
H5A H -0.085(6) 0.3928(17) -0.115(4) 0.061 Uiso 0.50 1 d PD B -1
H5B H -0.076(6) 0.309(6) -0.034(2) 0.061 Uiso 0.50 1 d PD C -1
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'
Co Co 0.3494 0.9721 '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'
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
O2 C1 O1 124.0(6) . .
O2 C1 C2 120.0(6) . .
O1 C1 C2 116.0(6) . .
C3A C2 C7B 100.3(10) . .
C3B C2 C7B 118.3(9) . .
C3A C2 C7A 118.4(9) . .
C3B C2 C7A 102.1(9) . .
C3A C2 C1 118.8(8) . .
C3B C2 C1 117.8(8) . .
C7B C2 C1 123.4(7) . .
C7A C2 C1 122.5(7) . .
C4A C5 C6B 99.8(10) . .
C4A C5 C6A 119.6(9) . .
C6B C5 C4B 118.1(9) . .
C6A C5 C4B 101.8(10) . .
C4A C5 C8 118.9(8) . .
C6B C5 C8 124.1(7) . .
C6A C5 C8 121.2(7) . .
C4B C5 C8 117.7(8) . .
C2 C3A C4A 122.0(13) . .
C2 C3A H3A 119.0 . .
C4A C3A H3A 119.0 . .
C5 C4A C3A 120.1(13) . .
C5 C4A H4A 120.0 . .
C3A C4A H4A 120.0 . .
C6B C6A C5 65.5(10) . .
C6B C6A C7A 90.9(10) . .
C5 C6A C7A 120.6(10) . .
C6B C6A C9 120.8(12) . .
C5 C6A C9 127.6(9) . .
C7A C6A C9 111.5(11) . .
C5 C6A C7B 97.2(8) . .
C9 C6A C7B 127.8(10) . .
C7B C7A C6A 88.5(10) . .
C6A C7A C2 119.0(10) . .
C7B C7A C10 119.3(12) . .
C6A C7A C10 114.2(11) . .
C2 C7A C10 126.7(10) . .
C2 C7A C6B 95.5(8) . .
C10 C7A C6B 128.5(9) . .
C2 C3B C4B 121.0(13) . .
C2 C3B H3B 119.5 . .
C4B C3B H3B 119.5 . .
C3B C4B C5 121.0(14) . .
C3B C4B H4B 119.5 . .
C5 C4B H4B 119.5 . .
C6A C6B C5 65.8(9) . .
C6A C6B C7B 90.5(11) . .
C5 C6B C7B 120.7(11) . .
C6A C6B C10 113.5(12) . 7
C5 C6B C10 126.5(10) . 7
C7B C6B C10 112.7(11) . 7
C5 C6B C7A 97.3(9) . .
C10 C6B C7A 123.8(10) 7 .
C7A C7B C6B 90.1(11) . .
C2 C7B C6B 120.3(10) . .
C7A C7B C9 115.1(11) . 7
C2 C7B C9 125.8(9) . 7
C6B C7B C9 113.9(11) . 7
C2 C7B C6A 98.3(9) . .
C9 C7B C6A 125.4(9) 7 .
O4 C8 O3 125.7(6) . .
O4 C8 C5 114.6(6) . .
O3 C8 C5 119.7(6) . .
C7B C9 C12 105.1(10) 7 .
C7B C9 C6A 105.2(9) 7 .
C12 C9 C6A 106.7(9) . .
C7B C9 H9 113.1 7 .
C12 C9 H9 113.1 . .
C6A C9 H9 113.1 . .
C7A C10 C6B 106.7(10) . 7
C7A C10 C11 106.5(10) . .
C6B C10 C11 103.5(9) 7 .
C7A C10 H10 113.1 . .
C6B C10 H10 113.1 7 .
C11 C10 H10 113.1 . .
C12 C11 C16 120.0 . .
C12 C11 C10 112.9(7) . .
C16 C11 C10 127.0(7) . .
C11 C12 C13 120.0 . .
C11 C12 C9 113.2(7) . .
C13 C12 C9 126.7(7) . .
C14 C13 C12 120.0 . .
C14 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C15 C14 C13 120.0 . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C14 C15 C16 120.0 . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
C15 C16 C11 120.0 . .
C15 C16 H16 120.0 . .
C11 C16 H16 120.0 . .
C1 O1 Co1 126.2(5) . .
C1 O2 Co2 158.1(6) . .
C8 O3 Co2 147.6(6) . 3_545
C8 O4 Co1 133.6(5) . 3_545
Co2 O5 H5A 103.8(12) . .
Co2 O5 H5B 103.9(12) . .
H5A O5 H5B 114.7(14) . .
C17 O6 Co2 130(2) . .
C18 N1 C17 119.3(7) . .
C18 N1 C19 119.6(7) . .
C17 N1 C19 119.7(7) . .
O6 C17 N1 137(2) . .
O6 C17 H17 111.3 . .
N1 C17 H17 111.3 . .
N1 C18 H18A 109.5 . .
N1 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
N1 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N1 C19 H19A 109.5 . .
N1 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
N1 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O4 Co1 O4 105.7(4) 4 3_455
O4 Co1 O1 98.2(3) 4 .
O4 Co1 O1 129.3(2) 3_455 .
O4 Co1 O1 129.3(2) 4 2
O4 Co1 O1 98.2(3) 3_455 2
O1 Co1 O1 100.0(3) . 2
O6 Co2 O6 180.000(2) . 5_565
O6 Co2 O2 93.8(8) . .
O6 Co2 O2 86.2(8) 5_565 .
O6 Co2 O2 86.2(8) . 5_565
O6 Co2 O2 93.8(8) 5_565 5_565
O2 Co2 O2 180.0 . 5_565
O6 Co2 O3 100.3(9) . 3_455
O6 Co2 O3 79.7(9) 5_565 3_455
O2 Co2 O3 95.7(2) . 3_455
O2 Co2 O3 84.3(2) 5_565 3_455
O6 Co2 O3 79.7(9) . 7
O6 Co2 O3 100.3(9) 5_565 7
O2 Co2 O3 84.3(2) . 7
O2 Co2 O3 95.7(2) 5_565 7
O3 Co2 O3 180.0(5) 3_455 7
O6 Co2 O5 17.4(8) . 5_565
O6 Co2 O5 162.6(8) 5_565 5_565
O2 Co2 O5 83.1(5) . 5_565
O2 Co2 O5 96.9(5) 5_565 5_565
O3 Co2 O5 87.8(5) 3_455 5_565
O3 Co2 O5 92.2(5) 7 5_565
O6 Co2 O5 162.6(8) . .
O6 Co2 O5 17.4(8) 5_565 .
O2 Co2 O5 96.9(5) . .
O2 Co2 O5 83.1(5) 5_565 .
O3 Co2 O5 92.2(5) 3_455 .
O3 Co2 O5 87.8(5) 7 .
O5 Co2 O5 180.000(1) 5_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.209(8) .
C1 O1 1.245(8) .
C1 C2 1.501(9) .
C2 C3A 1.360(17) .
C2 C3B 1.387(17) .
C2 C7B 1.404(14) .
C2 C7A 1.434(14) .
C5 C4A 1.372(17) .
C5 C6B 1.394(14) .
C5 C6A 1.398(15) .
C5 C4B 1.403(18) .
C5 C8 1.531(8) .
C3A C4A 1.42(2) .
C3A H3A 0.9300 .
C4A H4A 0.9300 .
C6A C6B 1.150(17) .
C6A C7A 1.420(16) .
C6A C9 1.544(16) .
C6A C7B 1.826(16) .
C7A C7B 1.185(17) .
C7A C10 1.489(18) .
C7A C6B 1.841(17) .
C3B C4B 1.39(2) .
C3B H3B 0.9300 .
C4B H4B 0.9300 .
C6B C7B 1.407(16) .
C6B C10 1.520(17) 7
C7B C9 1.491(17) 7
C8 O4 1.222(9) .
C8 O3 1.227(9) .
C9 C7B 1.491(17) 7
C9 C12 1.534(14) .
C9 H9 0.9800 .
C10 C6B 1.520(17) 7
C10 C11 1.549(13) .
C10 H10 0.9800 .
C11 C12 1.3900 .
C11 C16 1.3900 .
C12 C13 1.3900 .
C13 C14 1.3900 .
C13 H13 0.9300 .
C14 C15 1.3900 .
C14 H14 0.9300 .
C15 C16 1.3900 .
C15 H15 0.9300 .
C16 H16 0.9300 .
O1 Co1 1.939(5) .
O2 Co2 2.070(5) .
O3 Co2 2.079(5) 3_545
O4 Co1 1.925(5) 3_545
O5 Co2 2.096(16) .
O5 H5A 0.950(5) .
O5 H5B 0.949(5) .
O6 C17 1.186(10) .
O6 Co2 2.02(2) .
N1 C18 1.269(16) .
N1 C17 1.269(16) .
N1 C19 1.270(16) .
C17 H17 0.9300 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
Co1 O4 1.925(5) 4
Co1 O4 1.925(5) 3_455
Co1 O1 1.939(5) 2
Co2 O6 2.02(2) 5_565
Co2 O2 2.070(5) 5_565
Co2 O3 2.079(5) 3_455
Co2 O3 2.079(5) 7
Co2 O5 2.096(16) 5_565
