#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:14:15 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224207 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/91/7049142.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_7049142
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_sum            'C39 H54 Br Co N10 O3'
_chemical_formula_weight         849.76
_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                   15.5579(15)
_cell_length_b                   15.5579(15)
_cell_length_c                   12.1716(17)
_cell_measurement_reflns_used    9711
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.25
_cell_volume                     2551.4(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 0.885
_diffrn_measured_fraction_theta_max 0.887
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.885
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43477
_diffrn_reflns_point_group_measured_fraction_full 0.885
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.858
_diffrn_reflns_theta_min         1.673
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS,Bruker(2000)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0556
_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)+(0.1294P)²+0.7003P] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1965
_refine_ls_wR_factor_ref         0.2006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2312
_reflns_number_total             2927
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00739c2.cif
_cod_data_source_block           msn357
_cod_depositor_comments
'Adding full bibliography for 7049140--7049143.cif.'
_cod_original_cell_volume        2551.4(6)
_cod_database_code               7049142
_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           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
Br1 Br 0.6667 0.3333 0.81775(6) 0.0221(3) Uani 1 3 d S T P
Co1 Co 0.6667 0.3333 0.38737(8) 0.0152(3) Uani 1 3 d S T P
N1 N 0.7339(3) 0.4800(3) 0.3279(3) 0.0171(8) Uani 1 1 d . . .
O1 O 1.0446(2) 0.4653(3) 0.7510(3) 0.0262(8) Uani 1 1 d . . .
C1 C 0.7238(3) 0.4378(3) 0.1389(3) 0.0207(9) Uani 1 1 d . . .
H1A H 0.7019 0.4451 0.0648 0.025 Uiso 1 1 calc R U .
H1B H 0.7953 0.4593 0.1354 0.025 Uiso 1 1 calc R U .
N2 N 0.7965(3) 0.4226(3) 0.4998(3) 0.0174(8) Uani 1 1 d . . .
C2 C 0.7068(3) 0.5023(3) 0.2213(3) 0.0189(9) Uani 1 1 d . . .
H2A H 0.7491 0.5736 0.2033 0.023 Uiso 1 1 calc R U .
H2B H 0.6365 0.4855 0.2209 0.023 Uiso 1 1 calc R U .
N3 N 0.8881(3) 0.3391(3) 0.7875(3) 0.0214(8) Uani 1 1 d . . .
H3B H 0.8254 0.3128 0.7687 0.032 Uiso 1 1 calc R U .
C3 C 0.8085(3) 0.5485(3) 0.3790(4) 0.0191(9) Uani 1 1 d . . .
H3A H 0.8398 0.6153 0.3542 0.023 Uiso 1 1 calc R U .
C4 C 0.8447(3) 0.5215(3) 0.4766(3) 0.0178(9) Uani 1 1 d . . .
N4 N 0.6667 0.3333 0.1744(5) 0.0183(13) Uani 1 3 d S T P
C5 C 0.9251(4) 0.5903(3) 0.5361(4) 0.0265(10) Uani 1 1 d . . .
H5 H 0.9556 0.6588 0.5187 0.032 Uiso 1 1 calc R U .
C6 C 0.9612(4) 0.5586(4) 0.6217(4) 0.0274(11) Uani 1 1 d . . .
H6 H 1.0177 0.6046 0.6624 0.033 Uiso 1 1 calc R U .
C7 C 0.8303(3) 0.3932(3) 0.5838(4) 0.0206(9) Uani 1 1 d . . .
H7A H 0.7966 0.3246 0.6020 0.025 Uiso 1 1 calc R U .
C8 C 0.9130(3) 0.4582(3) 0.6467(3) 0.0185(9) Uani 1 1 d . . .
C9 C 0.9531(3) 0.4208(3) 0.7356(4) 0.0202(9) Uani 1 1 d . . .
C10 C 0.9124(3) 0.2883(4) 0.8747(4) 0.0243(10) Uani 1 1 d . . .
C11 C 0.8155(4) 0.1941(4) 0.9019(4) 0.0298(11) Uani 1 1 d . . .
H11A H 0.7654 0.2115 0.9232 0.045 Uiso 1 1 calc R U .
H11B H 0.8264 0.1594 0.9629 0.045 Uiso 1 1 calc R U .
H11C H 0.7925 0.1507 0.8373 0.045 Uiso 1 1 calc R U .
C12 C 0.9514(4) 0.3556(4) 0.9757(4) 0.0324(12) Uani 1 1 d . . .
H12A H 1.0147 0.4149 0.9577 0.049 Uiso 1 1 calc R U .
H12B H 0.9612 0.3197 1.0360 0.049 Uiso 1 1 calc R U .
H12C H 0.9032 0.3753 0.9979 0.049 Uiso 1 1 calc R U .
C13 C 0.9890(4) 0.2627(4) 0.8329(5) 0.0365(13) Uani 1 1 d . . .
H13A H 0.9658 0.2257 0.7639 0.055 Uiso 1 1 calc R U .
H13B H 0.9985 0.2219 0.8876 0.055 Uiso 1 1 calc R U .
H13C H 1.0522 0.3239 0.8204 0.055 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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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 108.84(10) 3_665 2_655
N1 Co1 N1 108.84(10) 3_665 .
N1 Co1 N1 108.84(10) 2_655 .
N1 Co1 N2 74.62(13) 3_665 3_665
N1 Co1 N2 86.95(13) 2_655 3_665
N1 Co1 N2 160.84(14) . 3_665
N1 Co1 N2 86.95(13) 3_665 .
N1 Co1 N2 160.84(13) 2_655 .
N1 Co1 N2 74.62(13) . .
N2 Co1 N2 86.93(13) 3_665 .
N1 Co1 N2 160.84(13) 3_665 2_655
N1 Co1 N2 74.62(13) 2_655 2_655
N1 Co1 N2 86.95(13) . 2_655
N2 Co1 N2 86.93(13) 3_665 2_655
N2 Co1 N2 86.93(13) . 2_655
C3 N1 C2 119.0(4) . .
C3 N1 Co1 119.2(3) . .
C2 N1 Co1 121.2(3) . .
N4 C1 C2 108.9(4) . .
C7 N2 C4 117.3(4) . .
C7 N2 Co1 129.9(3) . .
C4 N2 Co1 112.8(3) . .
N1 C2 C1 105.2(3) . .
C9 N3 C10 125.4(4) . .
N1 C3 C4 118.4(4) . .
N2 C4 C5 122.8(4) . .
N2 C4 C3 114.8(4) . .
C5 C4 C3 122.3(4) . .
C1 N4 C1 111.8(3) . 3_665
C1 N4 C1 111.8(3) . 2_655
C1 N4 C1 111.8(3) 3_665 2_655
C4 C5 C6 119.4(4) . .
C5 C6 C8 118.6(4) . .
N2 C7 C8 123.4(4) . .
C6 C8 C7 118.5(4) . .
C6 C8 C9 119.9(4) . .
C7 C8 C9 121.5(4) . .
O1 C9 N3 124.9(4) . .
O1 C9 C8 118.2(4) . .
N3 C9 C8 116.8(4) . .
N3 C10 C13 110.1(4) . .
N3 C10 C11 106.0(4) . .
C13 C10 C11 110.4(4) . .
N3 C10 C12 109.2(4) . .
C13 C10 C12 110.7(4) . .
C11 C10 C12 110.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.107(3) 3_665
Co1 N1 2.107(3) 2_655
Co1 N1 2.107(3) .
Co1 N2 2.253(3) 3_665
Co1 N2 2.253(4) .
Co1 N2 2.253(3) 2_655
N1 C3 1.278(5) .
N1 C2 1.459(5) .
O1 C9 1.247(5) .
C1 N4 1.475(5) .
C1 C2 1.531(6) .
N2 C7 1.331(6) .
N2 C4 1.363(6) .
N3 C9 1.323(6) .
N3 C10 1.481(6) .
C3 C4 1.463(6) .
C4 C5 1.377(6) .
N4 C1 1.475(5) 3_665
N4 C1 1.475(5) 2_655
C5 C6 1.386(7) .
C6 C8 1.386(7) .
C7 C8 1.402(6) .
C8 C9 1.503(6) .
C10 C13 1.520(7) .
C10 C11 1.524(7) .
C10 C12 1.530(7) .
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 -0.018 650 114 ' '
