#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:14:15 +0100 (jue 07 de nov de 2019) $
#$Revision: 224207 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/91/7049140.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_7049140
loop_
_publ_author_name
'Klug, Christina M.'
'Ozumerzifon, Tarik J.'
'Bhowmick, Indrani'
'Livesay, Brooke N.'
'Rappé, Anthony K'
'Shores, Matthew P.'
_publ_section_title
;
 Anionic guest-dependent slow magnetic relaxation in Co(ii) tripodal
 iminopyridine complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9117
_journal_page_last               9126
_journal_paper_doi               10.1039/c9dt00739c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C39 H54 Co N10 O3, Cl [+ solvent]'
_chemical_formula_sum            'C39 H54 Cl Co N10 O3'
_chemical_formula_weight         805.30
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-12-02 deposited with the CCDC.    2019-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.23350(10)
_cell_length_b                   15.23350(10)
_cell_length_c                   12.5157(2)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.204
_cell_measurement_theta_min      2.24
_cell_volume                     2515.27(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.735
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_unetI/netI     0.1166
_diffrn_reflns_Laue_measured_fraction_full 0.735
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_number            17457
_diffrn_reflns_point_group_measured_fraction_full 0.735
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.204
_diffrn_reflns_theta_min         2.243
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS,Bruker(2000)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_platon_squeeze_details
;
;
_refine_diff_density_max         1.297
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0667
_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)+(0.1211P)²] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2371
_reflns_number_total             3608
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00739c2.cif
_cod_data_source_block           msn335
_cod_depositor_comments
'Adding full bibliography for 7049140--7049143.cif.'
_cod_database_code               7049140
_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. 
;
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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 0.6667 0.3333 0.61977(6) 0.0154(2) Uani 1 3 d S T P
N4 N 0.6667 0.3333 0.8254(4) 0.0187(9) Uani 1 3 d S T P
O1 O 0.5348(2) -0.04132(18) 0.2534(2) 0.0271(6) Uani 1 1 d . . .
C1 C 0.7267(3) 0.2868(3) 0.8602(3) 0.0219(7) Uani 1 1 d . . .
H1A H 0.7056 0.2580 0.9328 0.026 Uiso 1 1 calc R U .
H1B H 0.7996 0.3386 0.8624 0.026 Uiso 1 1 calc R U .
Cl1 Cl 0.6667 0.3333 0.20744(14) 0.0269(4) Uani 1 3 d S T P
N1 N 0.7363(2) 0.2516(2) 0.6763(2) 0.0176(6) Uani 1 1 d . . .
C2 C 0.7093(3) 0.2029(3) 0.7811(3) 0.0200(7) Uani 1 1 d . . .
H2A H 0.7526 0.1736 0.7992 0.024 Uiso 1 1 calc R U .
H2B H 0.6375 0.1481 0.7822 0.024 Uiso 1 1 calc R U .
N2 N 0.5748(2) 0.2015(2) 0.5086(2) 0.0170(6) Uani 1 1 d . . .
C3 C 0.8102(2) 0.2565(2) 0.6251(3) 0.0191(7) Uani 1 1 d . . .
H3 H 0.8415 0.2193 0.6481 0.023 Uiso 1 1 calc R U .
N3 N 0.6615(2) 0.1202(2) 0.2216(2) 0.0219(6) Uani 1 1 d . . .
H4 H 0.6866 0.1838 0.2412 0.026 Uiso 1 1 calc R U .
C4 C 0.4742(2) 0.1529(2) 0.5292(3) 0.0187(7) Uani 1 1 d . . .
C5 C 0.4040(3) 0.0740(3) 0.4680(3) 0.0257(8) Uani 1 1 d . . .
H5 H 0.3338 0.0432 0.4842 0.031 Uiso 1 1 calc R U .
C6 C 0.4361(3) 0.0400(3) 0.3834(3) 0.0247(7) Uani 1 1 d . . .
H6 H 0.3888 -0.0156 0.3414 0.030 Uiso 1 1 calc R U .
C7 C 0.5396(3) 0.0886(2) 0.3601(3) 0.0202(7) Uani 1 1 d . . .
C8 C 0.6054(2) 0.1694(2) 0.4248(3) 0.0194(7) Uani 1 1 d . . .
H8 H 0.6757 0.2035 0.4085 0.023 Uiso 1 1 calc R U .
C9 C 0.5780(3) 0.0498(2) 0.2723(3) 0.0197(7) Uani 1 1 d . . .
C10 C 0.7148(3) 0.0985(3) 0.1347(3) 0.0293(8) Uani 1 1 d . . .
C11 C 0.6449(4) 0.0564(3) 0.0372(3) 0.0423(11) Uani 1 1 d . . .
H11A H 0.5855 -0.0088 0.0556 0.064 Uiso 1 1 calc R U .
H11B H 0.6816 0.0469 -0.0219 0.064 Uiso 1 1 calc R U .
H11C H 0.6229 0.1042 0.0155 0.064 Uiso 1 1 calc R U .
C12 C 0.7435(4) 0.0220(4) 0.1716(5) 0.0493(13) Uani 1 1 d . . .
H12A H 0.6826 -0.0451 0.1755 0.074 Uiso 1 1 calc R U .
H12B H 0.7750 0.0413 0.2424 0.074 Uiso 1 1 calc R U .
H12C H 0.7916 0.0202 0.1209 0.074 Uiso 1 1 calc R U .
C13 C 0.8085(3) 0.1997(3) 0.1094(4) 0.0344(9) Uani 1 1 d . . .
H13A H 0.8507 0.1893 0.0576 0.052 Uiso 1 1 calc R U .
H13B H 0.8472 0.2290 0.1751 0.052 Uiso 1 1 calc R U .
H13C H 0.7878 0.2459 0.0792 0.052 Uiso 1 1 calc R U .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N1 Co1 N1 109.46(8) . 2_655
N1 Co1 N1 109.46(8) . 3_665
N1 Co1 N1 109.46(8) 2_655 3_665
N1 Co1 N2 87.28(10) . .
N1 Co1 N2 159.53(11) 2_655 .
N1 Co1 N2 74.09(11) 3_665 .
N1 Co1 N2 74.09(11) . 2_655
N1 Co1 N2 87.28(10) 2_655 2_655
N1 Co1 N2 159.53(11) 3_665 2_655
N2 Co1 N2 86.14(10) . 2_655
N1 Co1 N2 159.53(11) . 3_665
N1 Co1 N2 74.09(10) 2_655 3_665
N1 Co1 N2 87.28(10) 3_665 3_665
N2 Co1 N2 86.13(10) . 3_665
N2 Co1 N2 86.13(10) 2_655 3_665
C1 N4 C1 111.7(2) . 3_665
C1 N4 C1 111.7(2) . 2_655
C1 N4 C1 111.7(2) 3_665 2_655
N4 C1 C2 108.7(3) . .
C3 N1 C2 120.1(3) . .
C3 N1 Co1 119.2(2) . .
C2 N1 Co1 120.1(2) . .
N1 C2 C1 105.6(3) . .
C8 N2 C4 117.2(3) . .
C8 N2 Co1 129.3(2) . .
C4 N2 Co1 113.4(2) . .
N1 C3 C4 118.9(3) . 2_655
C9 N3 C10 124.8(3) . .
N2 C4 C5 123.1(3) . .
N2 C4 C3 114.2(3) . 3_665
C5 C4 C3 122.7(3) . 3_665
C6 C5 C4 119.5(3) . .
C5 C6 C7 118.8(3) . .
C8 C7 C6 118.0(3) . .
C8 C7 C9 121.6(3) . .
C6 C7 C9 120.3(3) . .
N2 C8 C7 123.5(3) . .
O1 C9 N3 124.8(3) . .
O1 C9 C7 119.6(3) . .
N3 C9 C7 115.6(3) . .
N3 C10 C12 110.4(3) . .
N3 C10 C13 105.4(3) . .
C12 C10 C13 111.1(4) . .
N3 C10 C11 109.4(3) . .
C12 C10 C11 109.3(4) . .
C13 C10 C11 111.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.121(3) .
Co1 N1 2.121(3) 2_655
Co1 N1 2.121(3) 3_665
Co1 N2 2.262(3) .
Co1 N2 2.262(3) 2_655
Co1 N2 2.262(3) 3_665
N4 C1 1.476(4) .
N4 C1 1.476(4) 3_665
N4 C1 1.476(4) 2_655
O1 C9 1.226(4) .
C1 C2 1.531(5) .
N1 C3 1.264(4) .
N1 C2 1.461(4) .
N2 C8 1.335(4) .
N2 C4 1.353(4) .
C3 C4 1.475(5) 2_655
N3 C9 1.344(4) .
N3 C10 1.490(5) .
C4 C5 1.374(5) .
C4 C3 1.475(5) 3_665
C5 C6 1.371(5) .
C6 C7 1.397(5) .
C7 C8 1.394(5) .
C7 C9 1.499(5) .
C10 C12 1.507(6) .
C10 C13 1.521(6) .
C10 C11 1.534(6) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.013 641 70 ' '
