#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:45:54 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180154 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/50/7105040.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_7105040
loop_
_publ_author_name
'Zhang, Zhan'
'Dolphin, David'
_publ_section_title
;
 A triple-stranded helicate and mesocate from the same metal and
 ligand.
;
_journal_issue                   45
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6931
_journal_page_last               6933
_journal_paper_doi               10.1039/b913231g
_journal_year                    2009
_chemical_formula_sum            'C81 H90 Co2 N12'
_chemical_formula_weight         1349.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           176
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2009-07-23 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.0431(8)
_cell_length_b                   15.0431(8)
_cell_length_c                   24.400(2)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    173.0(1)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.27
_cell_volume                     4781.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            45184
_diffrn_reflns_theta_full        27.80
_diffrn_reflns_theta_max         27.80
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3875
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0332
_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)+(0.0499P)²+0.7354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                3252
_reflns_number_total             3875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b913231g.txt
_cod_data_source_block           CoMeso
_cod_original_sg_symbol_H-M      P63/m
_cod_database_code               7105040
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
'-y, 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
C1 C 0.58775(9) 0.40236(10) 0.49123(5) 0.0262(3) Uani 1 1 d . A .
H1 H 0.5459 0.3344 0.4780 0.031 Uiso 1 1 calc R . .
C2 C 0.59677(10) 0.49116(11) 0.46510(5) 0.0294(3) Uani 1 1 d . . .
C3 C 0.66232(10) 0.57351(10) 0.49692(5) 0.0294(3) Uani 1 1 d . A .
C4 C 0.69346(10) 0.53282(9) 0.54187(5) 0.0244(3) Uani 1 1 d . . .
C5 C 0.76186(10) 0.58685(10) 0.58319(5) 0.0257(3) Uani 1 1 d . A .
H5 H 0.7883 0.6589 0.5836 0.031 Uiso 1 1 calc R . .
C6 C 0.79652(9) 0.54779(9) 0.62440(5) 0.0225(2) Uani 1 1 d . . .
C7 C 0.86626(9) 0.60295(9) 0.66740(5) 0.0257(3) Uani 1 1 d . A .
H7 H 0.8987 0.6748 0.6736 0.031 Uiso 1 1 calc R . .
C8 C 0.87826(9) 0.53328(9) 0.69850(4) 0.0225(2) Uani 1 1 d . . .
C9 C 0.81507(9) 0.43646(9) 0.67369(4) 0.0212(2) Uani 1 1 d . A .
H9 H 0.8083 0.3738 0.6867 0.025 Uiso 1 1 calc R . .
C10 C 0.94084(13) 0.55157(14) 0.7500 0.0251(4) Uani 1 2 d S . .
H10A H 0.9987 0.6232 0.7500 0.030 Uiso 1 2 calc SR . .
H10B H 0.9700 0.5054 0.7500 0.030 Uiso 1 2 calc SR . .
C11A C 0.54598(12) 0.49052(14) 0.41182(5) 0.0400(4) Uani 0.746(5) 1 d PD A 1
H11A H 0.5503 0.5578 0.4066 0.048 Uiso 0.746(5) 1 calc PR A 1
H11B H 0.4725 0.4372 0.4133 0.048 Uiso 0.746(5) 1 calc PR A 1
C12A C 0.5961(2) 0.4694(3) 0.36369(8) 0.0654(10) Uani 0.746(5) 1 d PD A 1
H12A H 0.6672 0.5253 0.3601 0.098 Uiso 0.746(5) 1 calc PR A 1
H12B H 0.5582 0.4646 0.3301 0.098 Uiso 0.746(5) 1 calc PR A 1
H12C H 0.5952 0.4045 0.3697 0.098 Uiso 0.746(5) 1 calc PR A 1
C13 C 0.69515(13) 0.68454(12) 0.48829(6) 0.0423(4) Uani 1 1 d . . .
H13A H 0.7136 0.7201 0.5242 0.051 Uiso 1 1 calc R A .
H13B H 0.6365 0.6894 0.4734 0.051 Uiso 1 1 calc R . .
C14 C 0.78574(15) 0.73922(15) 0.44957(10) 0.0693(6) Uani 1 1 d . A .
H14A H 0.8442 0.7348 0.4640 0.104 Uiso 1 1 calc R . .
H14B H 0.8045 0.8115 0.4464 0.104 Uiso 1 1 calc R . .
H14C H 0.7670 0.7067 0.4134 0.104 Uiso 1 1 calc R . .
N1 N 0.64521(7) 0.42604(8) 0.53658(4) 0.0223(2) Uani 1 1 d . A .
N2 N 0.76580(7) 0.44413(7) 0.62951(4) 0.0193(2) Uani 1 1 d . A .
Co1 Co 0.6667 0.3333 0.583235(10) 0.01788(9) Uani 1 3 d S . .
C11B C 0.54598(12) 0.49052(14) 0.41182(5) 0.0400(4) Uani 0.254(5) 1 d PD A 2
H11C H 0.5000 0.5186 0.4191 0.048 Uiso 0.254(5) 1 calc PR A 2
H11D H 0.6002 0.5389 0.3866 0.048 Uiso 0.254(5) 1 calc PR A 2
C12B C 0.4857(7) 0.3924(4) 0.3824(3) 0.070(3) Uani 0.254(5) 1 d PD A 2
H12D H 0.5301 0.3643 0.3730 0.104 Uiso 0.254(5) 1 calc PR A 2
H12E H 0.4574 0.4041 0.3488 0.104 Uiso 0.254(5) 1 calc PR A 2
H12F H 0.4294 0.3437 0.4059 0.104 Uiso 0.254(5) 1 calc PR A 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'
N N 0.0061 0.0033 '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'
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
N1 C1 C2 112.00(11) . . ?
N1 C1 H1 124.0 . . ?
C2 C1 H1 124.0 . . ?
C3 C2 C1 106.35(11) . . ?
C3 C2 C11A 128.81(13) . . ?
C1 C2 C11A 124.80(13) . . ?
C2 C3 C4 106.60(11) . . ?
C2 C3 C13 127.76(12) . . ?
C4 C3 C13 125.63(12) . . ?
C5 C4 N1 123.38(11) . . ?
C5 C4 C3 127.63(12) . . ?
N1 C4 C3 108.95(11) . . ?
C4 C5 C6 127.35(12) . . ?
C4 C5 H5 116.3 . . ?
C6 C5 H5 116.3 . . ?
C5 C6 N2 123.58(11) . . ?
C5 C6 C7 127.61(11) . . ?
N2 C6 C7 108.81(10) . . ?
C8 C7 C6 107.57(11) . . ?
C8 C7 H7 126.2 . . ?
C6 C7 H7 126.2 . . ?
C7 C8 C9 105.73(10) . . ?
C7 C8 C10 128.80(12) . . ?
C9 C8 C10 125.42(12) . . ?
N2 C9 C8 111.68(10) . . ?
N2 C9 H9 124.2 . . ?
C8 C9 H9 124.2 . . ?
C8 C10 C8 112.58(13) . 8_557 ?
C8 C10 H10A 109.1 . . ?
C8 C10 H10A 109.1 8_557 . ?
C8 C10 H10B 109.1 . . ?
C8 C10 H10B 109.1 8_557 . ?
H10A C10 H10B 107.8 . . ?
C2 C11A C12A 111.55(14) . . ?
C2 C11A H11A 109.3 . . ?
C12A C11A H11A 109.3 . . ?
C2 C11A H11B 109.3 . . ?
C12A C11A H11B 109.3 . . ?
H11A C11A H11B 108.0 . . ?
C3 C13 C14 113.39(14) . . ?
C3 C13 H13A 108.9 . . ?
C14 C13 H13A 108.9 . . ?
C3 C13 H13B 108.9 . . ?
C14 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C1 N1 C4 106.09(10) . . ?
C1 N1 Co1 127.50(9) . . ?
C4 N1 Co1 126.26(8) . . ?
C9 N2 C6 106.21(9) . . ?
C9 N2 Co1 127.60(8) . . ?
C6 N2 Co1 126.14(8) . . ?
N2 Co1 N2 89.75(4) 4_665 . ?
N2 Co1 N2 89.75(4) 4_665 3_655 ?
N2 Co1 N2 89.75(4) . 3_655 ?
N2 Co1 N1 87.85(4) 4_665 3_655 ?
N2 Co1 N1 176.17(4) . 3_655 ?
N2 Co1 N1 93.22(4) 3_655 3_655 ?
N2 Co1 N1 93.22(4) 4_665 4_665 ?
N2 Co1 N1 87.85(4) . 4_665 ?
N2 Co1 N1 176.17(4) 3_655 4_665 ?
N1 Co1 N1 89.30(4) 3_655 4_665 ?
N2 Co1 N1 176.17(4) 4_665 . ?
N2 Co1 N1 93.22(4) . . ?
N2 Co1 N1 87.85(4) 3_655 . ?
N1 Co1 N1 89.30(4) 3_655 . ?
N1 Co1 N1 89.30(4) 4_665 . ?
H12D C12B H12E 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
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
C1 N1 1.3380(15) . ?
C1 C2 1.4242(17) . ?
C1 H1 0.9500 . ?
C2 C3 1.3742(19) . ?
C2 C11A 1.5054(17) . ?
C3 C4 1.4433(16) . ?
C3 C13 1.5010(19) . ?
C4 C5 1.3783(17) . ?
C4 N1 1.3992(16) . ?
C5 C6 1.3909(16) . ?
C5 H5 0.9500 . ?
C6 N2 1.3928(15) . ?
C6 C7 1.4211(16) . ?
C7 C8 1.3770(17) . ?
C7 H7 0.9500 . ?
C8 C9 1.4166(16) . ?
C8 C10 1.5106(14) . ?
C9 N2 1.3454(14) . ?
C9 H9 0.9500 . ?
C10 C8 1.5106(14) 8_557 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11A C12A 1.512(3) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13 C14 1.518(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N1 Co1 1.9481(10) . ?
N2 Co1 1.9471(9) . ?
Co1 N2 1.9471(9) 4_665 ?
Co1 N2 1.9471(9) 3_655 ?
Co1 N1 1.9481(10) 3_655 ?
Co1 N1 1.9481(10) 4_665 ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.99(15) . . . . ?
N1 C1 C2 C11A 176.78(12) . . . . ?
C1 C2 C3 C4 0.87(14) . . . . ?
C11A C2 C3 C4 -176.78(13) . . . . ?
C1 C2 C3 C13 -178.19(13) . . . . ?
C11A C2 C3 C13 4.2(2) . . . . ?
C2 C3 C4 C5 177.37(12) . . . . ?
C13 C3 C4 C5 -3.6(2) . . . . ?
C2 C3 C4 N1 -0.51(14) . . . . ?
C13 C3 C4 N1 178.57(13) . . . . ?
N1 C4 C5 C6 2.0(2) . . . . ?
C3 C4 C5 C6 -175.56(12) . . . . ?
C4 C5 C6 N2 0.4(2) . . . . ?
C4 C5 C6 C7 -179.36(12) . . . . ?
C5 C6 C7 C8 179.95(12) . . . . ?
N2 C6 C7 C8 0.17(13) . . . . ?
C6 C7 C8 C9 -0.07(13) . . . . ?
C6 C7 C8 C10 -177.54(12) . . . . ?
C7 C8 C9 N2 -0.06(13) . . . . ?
C10 C8 C9 N2 177.52(11) . . . . ?
C7 C8 C10 C8 93.96(17) . . . 8_557 ?
C9 C8 C10 C8 -83.05(18) . . . 8_557 ?
C3 C2 C11A C12A 105.2(2) . . . . ?
C1 C2 C11A C12A -72.1(2) . . . . ?
C2 C3 C13 C14 -85.16(19) . . . . ?
C4 C3 C13 C14 95.96(17) . . . . ?
C2 C1 N1 C4 0.65(13) . . . . ?
C2 C1 N1 Co1 -175.10(8) . . . . ?
C5 C4 N1 C1 -178.08(11) . . . . ?
C3 C4 N1 C1 -0.09(13) . . . . ?
C5 C4 N1 Co1 -2.25(17) . . . . ?
C3 C4 N1 Co1 175.74(8) . . . . ?
C8 C9 N2 C6 0.16(12) . . . . ?
C8 C9 N2 Co1 -177.40(8) . . . . ?
C5 C6 N2 C9 -179.99(11) . . . . ?
C7 C6 N2 C9 -0.20(12) . . . . ?
C5 C6 N2 Co1 -2.38(16) . . . . ?
C7 C6 N2 Co1 177.41(8) . . . . ?
C9 N2 Co1 N2 1.24(9) . . . 4_665 ?
C6 N2 Co1 N2 -175.86(9) . . . 4_665 ?
C9 N2 Co1 N2 90.99(7) . . . 3_655 ?
C6 N2 Co1 N2 -86.11(11) . . . 3_655 ?
C9 N2 Co1 N1 -50.0(6) . . . 3_655 ?
C6 N2 Co1 N1 132.9(6) . . . 3_655 ?
C9 N2 Co1 N1 -91.99(9) . . . 4_665 ?
C6 N2 Co1 N1 90.91(9) . . . 4_665 ?
C9 N2 Co1 N1 178.83(9) . . . . ?
C6 N2 Co1 N1 1.73(9) . . . . ?
C1 N1 Co1 N2 -43.7(6) . . . 4_665 ?
C4 N1 Co1 N2 141.4(6) . . . 4_665 ?
C1 N1 Co1 N2 175.42(10) . . . . ?
C4 N1 Co1 N2 0.48(10) . . . . ?
C1 N1 Co1 N2 -94.95(10) . . . 3_655 ?
C4 N1 Co1 N2 90.11(10) . . . 3_655 ?
C1 N1 Co1 N1 -1.70(10) . . . 3_655 ?
C4 N1 Co1 N1 -176.64(9) . . . 3_655 ?
C1 N1 Co1 N1 87.61(8) . . . 4_665 ?
C4 N1 Co1 N1 -87.33(11) . . . 4_665 ?
