#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:53:20 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185367 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/91/7039198.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_7039198
loop_
_publ_author_name
'Switlicka-Olszewska, Anna'
'Palion-Gazda, Joanna'
'Klemens, Tomasz'
'Machura, Barbara'
'Vallejo, Julia'
'Cano, Joan'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Single-ion magnet behaviour in mononuclear and two-dimensional
 dicyanamide-containing cobalt(ii) complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10181
_journal_page_last               10193
_journal_paper_doi               10.1039/c6dt01160h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C44 H40 Co N14'
_chemical_formula_sum            'C44 H40 Co N14'
_chemical_formula_weight         823.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-10-20 deposited with the CCDC.
2016-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                92.904(5)
_cell_angle_beta                 96.747(5)
_cell_angle_gamma                115.860(6)
_cell_formula_units_Z            1
_cell_length_a                   9.4691(6)
_cell_length_b                   9.6862(6)
_cell_length_c                   12.6826(7)
_cell_measurement_reflns_used    3257
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9850
_cell_measurement_theta_min      4.0120
_cell_volume                     1032.73(12)
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A Ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9158
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         3.744
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.78341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       needle
_exptl_crystal_F_000             429
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0441P)²+0.0896P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3019
_reflns_number_total             3652
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01160h2.cif
_cod_data_source_block           A12a
_cod_depositor_comments
'Adding full bibliography for 7039197--7039200.cif.'
_cod_database_code               7039198
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.5000 0.0000 0.5000 0.03801(13) Uani 1 2 d S . P
N1 N 0.57488(19) -0.06585(19) 0.35990(11) 0.0438(4) Uani 1 1 d . . .
N2 N 0.73016(19) -0.0410(2) 0.23897(12) 0.0481(4) Uani 1 1 d . . .
N3 N 0.74857(18) 0.12372(19) 0.56324(12) 0.0431(4) Uani 1 1 d . . .
N4 N 0.9880(2) 0.3133(2) 0.61680(14) 0.0539(5) Uani 1 1 d . . .
N97 N 0.8445(5) -0.3727(4) 0.6465(4) 0.1553(16) Uani 1 1 d . . .
N98 N 0.5840(4) -0.3884(3) 0.6265(3) 0.1074(9) Uani 1 1 d . . .
N99 N 0.4912(2) -0.2074(2) 0.56047(13) 0.0502(4) Uani 1 1 d . . .
C1 C 0.5425(3) -0.2085(2) 0.31269(15) 0.0478(5) Uani 1 1 d . . .
H1 H 0.4667 -0.3015 0.3296 0.057 Uiso 1 1 calc R U .
C2 C 0.6367(3) -0.1944(3) 0.23791(16) 0.0517(5) Uani 1 1 d . . .
H2 H 0.6375 -0.2742 0.1943 0.062 Uiso 1 1 calc R U .
C3 C 0.6889(3) 0.0315(2) 0.31309(15) 0.0493(5) Uani 1 1 d . . .
H3 H 0.7353 0.1382 0.3295 0.059 Uiso 1 1 calc R U .
C4 C 0.8572(3) 0.0321(3) 0.17420(17) 0.0654(7) Uani 1 1 d . . .
H4A H 0.9296 -0.0143 0.1829 0.078 Uiso 1 1 calc R U .
H4B H 0.9168 0.1410 0.2000 0.078 Uiso 1 1 calc R U .
C5 C 0.7276(3) 0.1061(3) 0.0187(2) 0.0678(7) Uani 1 1 d . . .
H5 H 0.7201 0.1789 0.0654 0.081 Uiso 1 1 calc R U .
C6 C 0.6723(4) 0.0920(4) -0.0880(2) 0.0843(9) Uani 1 1 d . . .
H6 H 0.6268 0.1545 -0.1127 0.101 Uiso 1 1 calc R U .
C7 C 0.6832(3) -0.0118(4) -0.1577(2) 0.0833(9) Uani 1 1 d . . .
H7 H 0.6468 -0.0200 -0.2302 0.100 Uiso 1 1 calc R U .
C8 C 0.7477(3) -0.1041(4) -0.1211(2) 0.0821(9) Uani 1 1 d . . .
H8 H 0.7549 -0.1762 -0.1686 0.099 Uiso 1 1 calc R U .
C9 C 0.8029(3) -0.0915(3) -0.0133(2) 0.0642(6) Uani 1 1 d . . .
H9 H 0.8466 -0.1555 0.0112 0.077 Uiso 1 1 calc R U .
C10 C 0.7936(2) 0.0150(3) 0.05758(15) 0.0472(5) Uani 1 1 d . . .
C11 C 0.8580(3) 0.0658(3) 0.57217(16) 0.0519(5) Uani 1 1 d . . .
H11 H 0.8341 -0.0378 0.5575 0.062 Uiso 1 1 calc R U .
C12 C 1.0043(3) 0.1804(3) 0.60513(18) 0.0594(6) Uani 1 1 d . . .
H12 H 1.0984 0.1710 0.6176 0.071 Uiso 1 1 calc R U .
C13 C 0.8321(2) 0.2728(2) 0.59063(16) 0.0485(5) Uani 1 1 d . . .
H13 H 0.7888 0.3424 0.5918 0.058 Uiso 1 1 calc R U .
C14 C 1.1121(3) 0.4671(3) 0.6590(2) 0.0674(7) Uani 1 1 d . . .
H14A H 1.0721 0.5424 0.6463 0.081 Uiso 1 1 calc R U .
H14B H 1.2021 0.4916 0.6214 0.081 Uiso 1 1 calc R U .
C15 C 1.1666(2) 0.4784(3) 0.77752(18) 0.0535(5) Uani 1 1 d . . .
C16 C 1.3236(3) 0.5654(3) 0.8205(2) 0.0638(6) Uani 1 1 d . . .
H16 H 1.3971 0.6163 0.7762 0.077 Uiso 1 1 calc R U .
C17 C 1.3732(3) 0.5781(3) 0.9289(2) 0.0777(8) Uani 1 1 d . . .
H17 H 1.4799 0.6377 0.9567 0.093 Uiso 1 1 calc R U .
C18 C 1.2689(4) 0.5050(3) 0.9952(2) 0.0765(7) Uani 1 1 d . . .
H18 H 1.3033 0.5142 1.0682 0.092 Uiso 1 1 calc R U .
C19 C 1.1128(3) 0.4179(3) 0.9541(2) 0.0775(7) Uani 1 1 d . . .
H19 H 1.0403 0.3671 0.9991 0.093 Uiso 1 1 calc R U .
C20 C 1.0620(3) 0.4046(3) 0.8465(2) 0.0721(7) Uani 1 1 d . . .
H20 H 0.9551 0.3447 0.8195 0.087 Uiso 1 1 calc R U .
C98 C 0.7254(4) -0.3732(3) 0.6331(2) 0.0780(8) Uani 1 1 d . . .
C99 C 0.5418(3) -0.2883(3) 0.58800(16) 0.0535(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
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'
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
N3 Co1 N3 180.0 . 2_656
N3 Co1 N1 86.01(6) . .
N3 Co1 N1 93.99(6) 2_656 .
N3 Co1 N1 93.99(6) . 2_656
N3 Co1 N1 86.01(6) 2_656 2_656
N1 Co1 N1 180.0 . 2_656
N3 Co1 N99 89.36(7) . 2_656
N3 Co1 N99 90.64(6) 2_656 2_656
N1 Co1 N99 92.71(6) . 2_656
N1 Co1 N99 87.29(6) 2_656 2_656
N3 Co1 N99 90.64(6) . .
N3 Co1 N99 89.36(7) 2_656 .
N1 Co1 N99 87.28(6) . .
N1 Co1 N99 92.71(6) 2_656 .
N99 Co1 N99 180.0 2_656 .
C3 N1 C1 104.87(16) . .
C3 N1 Co1 123.63(13) . .
C1 N1 Co1 130.52(13) . .
C3 N2 C2 106.81(17) . .
C3 N2 C4 126.4(2) . .
C2 N2 C4 126.77(19) . .
C13 N3 C11 104.85(17) . .
C13 N3 Co1 127.74(14) . .
C11 N3 Co1 127.04(14) . .
C13 N4 C12 106.49(18) . .
C13 N4 C14 126.3(2) . .
C12 N4 C14 127.01(19) . .
C98 N98 C99 122.8(3) . .
C99 N99 Co1 155.32(18) . .
C2 C1 N1 109.94(19) . .
C2 C1 H1 125.0 . .
N1 C1 H1 125.0 . .
C1 C2 N2 106.39(19) . .
C1 C2 H2 126.8 . .
N2 C2 H2 126.8 . .
N1 C3 N2 111.99(19) . .
N1 C3 H3 124.0 . .
N2 C3 H3 124.0 . .
N2 C4 C10 112.37(17) . .
N2 C4 H4A 109.1 . .
C10 C4 H4A 109.1 . .
N2 C4 H4B 109.1 . .
C10 C4 H4B 109.1 . .
H4A C4 H4B 107.9 . .
C10 C5 C6 121.1(3) . .
C10 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
C7 C6 C5 120.6(3) . .
C7 C6 H6 119.7 . .
C5 C6 H6 119.7 . .
C6 C7 C8 119.5(2) . .
C6 C7 H7 120.3 . .
C8 C7 H7 120.3 . .
C7 C8 C9 120.3(3) . .
C7 C8 H8 119.8 . .
C9 C8 H8 119.8 . .
C10 C9 C8 120.3(3) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C5 C10 C9 118.1(2) . .
C5 C10 C4 121.3(2) . .
C9 C10 C4 120.6(2) . .
C12 C11 N3 110.1(2) . .
C12 C11 H11 124.9 . .
N3 C11 H11 124.9 . .
C11 C12 N4 106.53(19) . .
C11 C12 H12 126.7 . .
N4 C12 H12 126.7 . .
N3 C13 N4 112.03(19) . .
N3 C13 H13 124.0 . .
N4 C13 H13 124.0 . .
N4 C14 C15 111.96(19) . .
N4 C14 H14A 109.2 . .
C15 C14 H14A 109.2 . .
N4 C14 H14B 109.2 . .
C15 C14 H14B 109.2 . .
H14A C14 H14B 107.9 . .
C16 C15 C20 117.5(2) . .
C16 C15 C14 120.5(2) . .
C20 C15 C14 121.9(2) . .
C15 C16 C17 120.7(2) . .
C15 C16 H16 119.7 . .
C17 C16 H16 119.7 . .
C18 C17 C16 120.9(2) . .
C18 C17 H17 119.5 . .
C16 C17 H17 119.5 . .
C17 C18 C19 119.3(3) . .
C17 C18 H18 120.4 . .
C19 C18 H18 120.4 . .
C18 C19 C20 120.3(3) . .
C18 C19 H19 119.8 . .
C20 C19 H19 119.8 . .
C19 C20 C15 121.3(2) . .
C19 C20 H20 119.4 . .
C15 C20 H20 119.4 . .
N97 C98 N98 172.1(4) . .
N99 C99 N98 172.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N3 2.1489(15) .
Co1 N3 2.1489(15) 2_656
Co1 N1 2.1546(15) .
Co1 N1 2.1546(15) 2_656
Co1 N99 2.1574(18) 2_656
Co1 N99 2.1575(18) .
N1 C3 1.314(2) .
N1 C1 1.366(3) .
N2 C3 1.337(3) .
N2 C2 1.357(3) .
N2 C4 1.474(3) .
N3 C13 1.312(3) .
N3 C11 1.374(3) .
N4 C13 1.345(3) .
N4 C12 1.365(3) .
N4 C14 1.460(3) .
N97 C98 1.118(4) .
N98 C98 1.274(4) .
N98 C99 1.295(3) .
N99 C99 1.133(3) .
C1 C2 1.349(3) .
C1 H1 0.9300 .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 C10 1.502(3) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C10 1.365(3) .
C5 C6 1.370(4) .
C5 H5 0.9300 .
C6 C7 1.351(4) .
C6 H6 0.9300 .
C7 C8 1.356(4) .
C7 H7 0.9300 .
C8 C9 1.384(4) .
C8 H8 0.9300 .
C9 C10 1.373(3) .
C9 H9 0.9300 .
C11 C12 1.343(3) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 C15 1.513(3) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.373(3) .
C15 C20 1.381(3) .
C16 C17 1.381(4) .
C16 H16 0.9300 .
C17 C18 1.353(4) .
C17 H17 0.9300 .
C18 C19 1.362(4) .
C18 H18 0.9300 .
C19 C20 1.372(4) .
C19 H19 0.9300 .
C20 H20 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C13 H13 N97 0.93 2.61 3.418(4) 145.4 1_565
C14 H14A N97 0.97 2.62 3.495(4) 150.1 1_565
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
C3 N1 C1 C2 -0.4(2)
Co1 N1 C1 C2 -169.11(14)
N1 C1 C2 N2 0.5(2)
C3 N2 C2 C1 -0.3(2)
C4 N2 C2 C1 177.42(19)
C1 N1 C3 N2 0.2(2)
Co1 N1 C3 N2 169.88(12)
C2 N2 C3 N1 0.1(2)
C4 N2 C3 N1 -177.66(18)
C3 N2 C4 C10 -113.7(2)
C2 N2 C4 C10 68.9(3)
C10 C5 C6 C7 -0.7(4)
C5 C6 C7 C8 0.9(4)
C6 C7 C8 C9 -0.4(4)
C7 C8 C9 C10 -0.3(4)
C6 C5 C10 C9 0.0(4)
C6 C5 C10 C4 178.8(2)
C8 C9 C10 C5 0.5(3)
C8 C9 C10 C4 -178.4(2)
N2 C4 C10 C5 78.1(3)
N2 C4 C10 C9 -103.0(3)
C13 N3 C11 C12 0.3(2)
Co1 N3 C11 C12 173.70(14)
N3 C11 C12 N4 -0.3(2)
C13 N4 C12 C11 0.2(2)
C14 N4 C12 C11 174.9(2)
C11 N3 C13 N4 -0.2(2)
Co1 N3 C13 N4 -173.51(12)
C12 N4 C13 N3 0.0(2)
C14 N4 C13 N3 -174.72(19)
C13 N4 C14 C15 104.5(3)
C12 N4 C14 C15 -69.1(3)
N4 C14 C15 C16 143.2(2)
N4 C14 C15 C20 -37.8(3)
C20 C15 C16 C17 -0.2(4)
C14 C15 C16 C17 178.9(2)
C15 C16 C17 C18 0.2(4)
C16 C17 C18 C19 0.0(4)
C17 C18 C19 C20 -0.1(4)
C18 C19 C20 C15 0.0(4)
C16 C15 C20 C19 0.1(4)
C14 C15 C20 C19 -178.9(3)
