#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:07:30 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228807 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/96/1549677.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_1549677
loop_
_publ_author_name
'Bhowmick, Indrani'
'Roehl, Andrew J.'
'Neilson, James R.'
'Rappé, Anthony K'
'Shores, Matthew P.'
_publ_section_title
;
 Slow magnetic relaxation in octahedral low-spin Ni(iii) complexes.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              6564
_journal_page_last               6571
_journal_paper_doi               10.1039/c7sc04482h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C10 H26 Co0.9 N9 Ni0.1 O15'
_chemical_formula_weight         571.29
_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-2013
_audit_update_record
;
2017-10-11 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                89.163(3)
_cell_angle_beta                 76.951(5)
_cell_angle_gamma                81.894(4)
_cell_formula_units_Z            1
_cell_length_a                   7.371(5)
_cell_length_b                   8.496(4)
_cell_length_c                   9.080(5)
_cell_measurement_reflns_used    15604
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.332
_cell_measurement_theta_min      2.303
_cell_volume                     548.3(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex 2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15604
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.303
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       block
_exptl_crystal_F_000             294.1
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.346
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2723
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0355
_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)+(0.0710P)²+0.3327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2589
_reflns_number_total             2723
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7sc04482h8.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1549676--1549679.cif.'
_cod_original_formula_sum        'C10 H26 Co0.90 N9 Ni0.10 O15'
_cod_database_code               1549677
_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           2013-4
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.0000 0.0000 0.01020(13) Uani 0.9 2 d S . P . .
Ni1 Ni 0.0000 0.0000 0.0000 0.01020(13) Uani 0.1 2 d S . P . .
O1 O -0.4396(2) 0.02869(19) 0.14016(18) 0.0226(3) Uani 1 1 d . . . . .
O3 O -0.18379(19) -0.14347(17) 0.05982(17) 0.0174(3) Uani 1 1 d . . . . .
O2 O -0.4507(2) -0.2259(2) 0.1402(2) 0.0290(4) Uani 1 1 d . . . . .
N1 N -0.1573(2) 0.1451(2) -0.10797(19) 0.0148(3) Uani 1 1 d . . . . .
H1 H -0.2851 0.1180 -0.0758 0.018 Uiso 1 1 calc R U . . .
N2 N -0.0836(2) 0.1267(2) 0.19059(19) 0.0166(3) Uani 1 1 d . . . . .
H2 H -0.2047 0.0957 0.2425 0.020 Uiso 1 1 calc R U . . .
N3 N -0.3647(2) -0.1110(2) 0.1157(2) 0.0185(4) Uani 1 1 d . . . . .
C2 C -0.2477(3) 0.3646(3) 0.0845(3) 0.0255(5) Uani 1 1 d . . . . .
H2A H -0.2745 0.4795 0.0946 0.031 Uiso 1 1 calc R U . . .
H2B H -0.3651 0.3224 0.1211 0.031 Uiso 1 1 calc R U . . .
C4 C 0.0522(3) 0.0735(3) 0.2869(2) 0.0217(4) Uani 1 1 d . . . . .
H4A H -0.0024 0.1054 0.3915 0.026 Uiso 1 1 calc R U . . .
H4B H 0.1665 0.1209 0.2532 0.026 Uiso 1 1 calc R U . . .
C5 C -0.0954(3) 0.1048(3) -0.2726(2) 0.0210(4) Uani 1 1 d . . . . .
H5A H 0.0156 0.1529 -0.3173 0.025 Uiso 1 1 calc R U . . .
H5B H -0.1943 0.1439 -0.3241 0.025 Uiso 1 1 calc R U . . .
C1 C -0.1736(3) 0.3196(2) -0.0818(3) 0.0212(4) Uani 1 1 d . . . . .
H1A H -0.2577 0.3748 -0.1399 0.025 Uiso 1 1 calc R U . . .
H1B H -0.0510 0.3534 -0.1170 0.025 Uiso 1 1 calc R U . . .
C3 C -0.1123(3) 0.3037(3) 0.1826(3) 0.0247(5) Uani 1 1 d . . . . .
H3A H 0.0079 0.3399 0.1424 0.030 Uiso 1 1 calc R U . . .
H3B H -0.1607 0.3483 0.2840 0.030 Uiso 1 1 calc R U . . .
N6 N 0.5000 0.0000 0.5000 0.0511(11) Uani 1 2 d DS U P . .
O8 O 0.6461(5) 0.0118(6) 0.4659(4) 0.0305(8) Uani 0.5 1 d D U P . .
O9 O 0.4435(6) -0.1567(5) 0.5205(5) 0.0357(8) Uani 0.5 1 d . . P . .
O7 O 0.3509(5) 0.0909(5) 0.5694(5) 0.0338(8) Uani 0.5 1 d . . P . .
O5 O 0.6888(4) 0.6367(3) 0.6736(2) 0.0528(6) Uani 1 1 d . . . . .
O6 O 0.6149(8) 0.6116(6) 0.4427(5) 0.0452(9) Uani 0.5 1 d . . P A 1
O4 O 0.7082(9) 0.4143(6) 0.5720(6) 0.0595(8) Uani 0.5 1 d . . P A 1
N4 N 0.6681(10) 0.5545(6) 0.5695(6) 0.0402(12) Uani 0.5 1 d . . P A 1
O4A O 0.9036(7) 0.4476(6) 0.5373(5) 0.0526(11) Uani 0.5 1 d . . P A 2
O6A O 0.7274(7) 0.6212(5) 0.4329(5) 0.0421(4) Uani 0.5 1 d . . P A 2
N4A N 0.7836(8) 0.5614(6) 0.5592(5) 0.0314(9) Uani 0.5 1 d . . P 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'
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'
Ni Ni 0.3393 1.1124 '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
O3 Co1 O3 180.0 2 .
O3 Co1 N1 94.75(8) 2 2
O3 Co1 N1 85.25(8) . 2
O3 Co1 N1 85.25(8) 2 .
O3 Co1 N1 94.75(8) . .
N1 Co1 N1 180.0 2 .
O3 Co1 N2 86.04(7) 2 .
O3 Co1 N2 93.96(7) . .
N1 Co1 N2 86.48(8) 2 .
N1 Co1 N2 93.52(8) . .
O3 Co1 N2 93.96(7) 2 2
O3 Co1 N2 86.04(7) . 2
N1 Co1 N2 93.52(8) 2 2
N1 Co1 N2 86.48(8) . 2
N2 Co1 N2 180.0 . 2
N3 O3 Co1 129.26(13) . .
C1 N1 C5 110.70(16) . .
C1 N1 Co1 118.84(13) . .
C5 N1 Co1 108.18(13) . .
C1 N1 H1 106.1 . .
C5 N1 H1 106.1 . .
Co1 N1 H1 106.1 . .
C4 N2 C3 110.15(17) . .
C4 N2 Co1 107.21(13) . .
C3 N2 Co1 118.86(14) . .
C4 N2 H2 106.7 . .
C3 N2 H2 106.7 . .
Co1 N2 H2 106.7 . .
O2 N3 O1 123.90(18) . .
O2 N3 O3 115.95(18) . .
O1 N3 O3 120.14(17) . .
C3 C2 C1 113.52(18) . .
C3 C2 H2A 108.9 . .
C1 C2 H2A 108.9 . .
C3 C2 H2B 108.9 . .
C1 C2 H2B 108.9 . .
H2A C2 H2B 107.7 . .
N2 C4 C5 107.36(17) . 2
N2 C4 H4A 110.2 . .
C5 C4 H4A 110.2 2 .
N2 C4 H4B 110.2 . .
C5 C4 H4B 110.2 2 .
H4A C4 H4B 108.5 . .
N1 C5 C4 107.05(16) . 2
N1 C5 H5A 110.3 . .
C4 C5 H5A 110.3 2 .
N1 C5 H5B 110.3 . .
C4 C5 H5B 110.3 2 .
H5A C5 H5B 108.6 . .
N1 C1 C2 111.62(17) . .
N1 C1 H1A 109.3 . .
C2 C1 H1A 109.3 . .
N1 C1 H1B 109.3 . .
C2 C1 H1B 109.3 . .
H1A C1 H1B 108.0 . .
N2 C3 C2 112.48(18) . .
N2 C3 H3A 109.1 . .
C2 C3 H3A 109.1 . .
N2 C3 H3B 109.1 . .
C2 C3 H3B 109.1 . .
H3A C3 H3B 107.8 . .
O8 N6 O8 180.0 . 2_656
O8 N6 O7 45.2(3) . 2_656
O8 N6 O7 134.8(3) 2_656 2_656
O8 N6 O7 134.8(3) . .
O8 N6 O7 45.2(3) 2_656 .
O7 N6 O7 180.0(3) 2_656 .
O8 N6 O9 60.3(3) . 2_656
O8 N6 O9 119.7(3) 2_656 2_656
O7 N6 O9 102.6(2) 2_656 2_656
O7 N6 O9 77.4(2) . 2_656
O8 N6 O9 119.7(3) . .
O8 N6 O9 60.3(3) 2_656 .
O7 N6 O9 77.4(2) 2_656 .
O7 N6 O9 102.6(2) . .
O9 N6 O9 180.0 2_656 .
O7 O8 N6 80.0(4) 2_656 .
O7 O8 O9 145.6(5) 2_656 2_656
N6 O8 O9 74.3(3) . 2_656
O8 O9 N6 45.4(2) 2_656 .
O8 O9 O7 91.4(3) 2_656 2_656
N6 O9 O7 47.22(19) . 2_656
O8 O7 N6 54.8(3) 2_656 .
O8 O7 O9 107.6(4) 2_656 2_656
N6 O7 O9 55.41(19) . 2_656
O4 N4 O5 119.2(5) . .
O4 N4 O6 115.5(5) . .
O5 N4 O6 125.2(5) . .
N4A O4A O4A 96.9(5) . 2_766
O4A N4A O5 134.5(5) . .
O4A N4A O6A 115.3(4) . .
O5 N4A O6A 110.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 1.9313(16) 2
Co1 O3 1.9313(16) .
Co1 N1 1.9747(18) 2
Co1 N1 1.9748(18) .
Co1 N2 1.9795(18) .
Co1 N2 1.9796(18) 2
O1 N3 1.237(2) .
O3 N3 1.306(2) .
O2 N3 1.229(2) .
N1 C1 1.489(3) .
N1 C5 1.491(3) .
N1 H1 0.9800 .
N2 C4 1.492(3) .
N2 C3 1.492(3) .
N2 H2 0.9800 .
C2 C3 1.516(3) .
C2 C1 1.520(3) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C4 C5 1.505(3) 2
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C4 1.505(3) 2
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
N6 O8 1.070(3) .
N6 O8 1.070(3) 2_656
N6 O7 1.290(4) 2_656
N6 O7 1.290(4) .
N6 O9 1.447(4) 2_656
N6 O9 1.447(4) .
O8 O7 0.930(5) 2_656
O8 O9 1.305(6) 2_656
O9 O8 1.305(6) 2_656
O9 O7 1.715(6) 2_656
O7 O8 0.930(5) 2_656
O7 O9 1.715(6) 2_656
O5 N4 1.233(5) .
O5 N4A 1.242(5) .
O6 N4 1.360(7) .
O4 N4 1.187(7) .
O4A N4A 1.201(6) .
O4A O4A 1.782(11) 2_766
O6A N4A 1.372(6) .
