#------------------------------------------------------------------------------
#$Date: 2023-05-05 03:21:07 +0300 (Fri, 05 May 2023) $
#$Revision: 283074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/11/7131144.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_7131144
loop_
_publ_author_name
'Landart-Gereka, Aritz'
'Quesada-Moreno, María Mar'
'Palacios, María A'
'Díaz-Ortega, Ismael F'
'Nojiri, Hiroyuki'
'Ozerov, Mykhaylo'
'Krzystek, J.'
'Colacio, Enrique'
_publ_section_title
;
 Pushing up the easy-axis magnetic anisotropy and relaxation times in
 trigonal prismatic CoII mononuclear SMMs by molecular
 structure design.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              952
_journal_page_last               955
_journal_paper_doi               10.1039/d2cc06012d
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C18 H27 Co1 N12 P1 S1, 2(Cl1 O4)'
_chemical_formula_sum            'C18 H27 Cl2 Co N12 O8 P S'
_chemical_formula_weight         732.37
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-04-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-28 deposited with the CCDC.	2022-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.1198(13)
_cell_length_b                   10.1198(13)
_cell_length_c                   16.131(2)
_cell_measurement_reflns_used    9440
_cell_measurement_temperature    99.9
_cell_measurement_theta_max      28.396
_cell_measurement_theta_min      2.324
_cell_volume                     1430.7(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24534
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.397
_diffrn_reflns_theta_min         2.324
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  0.7899
_exptl_absorpt_correction_T_min  0.6526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0926 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.8262.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             750
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1029 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(13)
_refine_ls_extinction_coef       0.013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2376
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0316
_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)+(0.0496P)²+0.8899P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                2256
_reflns_number_total             2376
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc06012d2.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
'Adding full bibliography for 7131143--7131144.cif.'
_cod_original_cell_volume        1430.7(4)
_cod_database_code               7131144
_shelxl_version_number           2014-3
_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_max   0.832
_shelx_estimated_absorpt_t_min   0.671
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O3A)
Uanis(O4) = Uanis(O4A)
3. Others
 Fixed Sof: O3(0.16667) O4A(0.16667) O3A(0.5) O4(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'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_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 0.6667 0.3333 0.30699(4) 0.01284(19) Uani 1 3 d S T P . .
S1 S 0.6667 0.3333 -0.02664(9) 0.0180(3) Uani 1 3 d S T P . .
P1 P 0.6667 0.3333 0.09218(9) 0.0126(3) Uani 1 3 d S T P . .
N1 N 0.6621(3) 0.1773(3) 0.13246(19) 0.0189(5) Uani 1 1 d . . . . .
N4 N 0.7183(3) -0.0269(3) 0.3906(2) 0.0199(5) Uani 1 1 d . . . . .
N3 N 0.7020(3) 0.1833(3) 0.38095(18) 0.0176(5) Uani 1 1 d . . . . .
C3 C 0.7011(3) 0.0690(4) 0.3394(2) 0.0161(6) Uani 1 1 d . . . . .
C1 C 0.6325(4) 0.0442(4) 0.0831(2) 0.0199(6) Uani 1 1 d . . . . .
H1A H 0.6212 0.0633 0.0246 0.030 Uiso 1 1 calc R U . . .
H1B H 0.5385 -0.0451 0.1025 0.030 Uiso 1 1 calc R U . . .
H1C H 0.7180 0.0253 0.0890 0.030 Uiso 1 1 calc R U . . .
N2 N 0.6789(3) 0.1733(3) 0.21686(17) 0.0159(5) Uani 1 1 d . . . . .
C2 C 0.6852(4) 0.0601(4) 0.24989(19) 0.0162(6) Uani 1 1 d . . . . .
H2 H 0.6798 -0.0217 0.2183 0.019 Uiso 1 1 calc R U . . .
C4 C 0.7185(4) 0.1574(4) 0.4630(2) 0.0214(6) Uani 1 1 d . . . . .
H4 H 0.7225 0.2198 0.5081 0.026 Uiso 1 1 calc R U . . .
C5 C 0.7283(4) 0.0282(4) 0.4697(2) 0.0224(7) Uani 1 1 d . . . . .
H5 H 0.7397 -0.0154 0.5194 0.027 Uiso 1 1 calc R U . . .
C6 C 0.7227(5) -0.1648(5) 0.3679(2) 0.0313(9) Uani 1 1 d . . . . .
H6A H 0.6184 -0.2515 0.3645 0.047 Uiso 1 1 calc R U . . .
H6B H 0.7797 -0.1857 0.4100 0.047 Uiso 1 1 calc R U . . .
H6C H 0.7731 -0.1497 0.3140 0.047 Uiso 1 1 calc R U . . .
Cl1 Cl 1.0000 0.0000 0.13945(11) 0.0189(3) Uani 1 3 d S T P . .
O2 O 1.0067(4) 0.1387(3) 0.1677(2) 0.0357(7) Uani 1 1 d . . . . .
O1 O 1.0000 0.0000 0.0503(3) 0.0273(9) Uani 1 3 d S T P . .
Cl2 Cl 0.3333 -0.3333 0.20974(10) 0.0231(3) Uani 1 3 d S T P . .
O3 O 0.3333 -0.3333 0.1262(9) 0.0365(13) Uani 0.5 3 d S T P A 1
O4A O 0.3333 -0.3333 0.2927(11) 0.064(2) Uani 0.5 3 d S T P A 2
O3A O 0.4807(7) -0.3043(7) 0.1749(5) 0.0365(13) Uani 0.5 1 d . . P A 2
O4 O 0.3340(11) -0.1992(11) 0.2429(6) 0.064(2) Uani 0.5 1 d . . P A 1
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'
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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N3 Co1 N3 90.86(11) . 3_655 ?
N3 Co1 N3 90.86(11) . 5_665 ?
N3 Co1 N3 90.86(11) 3_655 5_665 ?
N3 Co1 N2 128.16(11) . 3_655 ?
N3 Co1 N2 75.70(10) 5_665 5_665 ?
N3 Co1 N2 138.05(11) . 5_665 ?
N3 Co1 N2 75.70(10) 3_655 3_655 ?
N3 Co1 N2 75.70(10) . . ?
N3 Co1 N2 128.16(11) 3_655 5_665 ?
N3 Co1 N2 138.05(11) 3_655 . ?
N3 Co1 N2 128.16(11) 5_665 . ?
N3 Co1 N2 138.05(11) 5_665 3_655 ?
N2 Co1 N2 81.94(11) . 5_665 ?
N2 Co1 N2 81.94(11) . 3_655 ?
N2 Co1 N2 81.94(11) 3_655 5_665 ?
N1 P1 S1 112.66(11) 3_655 . ?
N1 P1 S1 112.66(11) 5_665 . ?
N1 P1 S1 112.66(11) . . ?
N1 P1 N1 106.10(12) . 3_655 ?
N1 P1 N1 106.10(12) 3_655 5_665 ?
N1 P1 N1 106.10(12) . 5_665 ?
C1 N1 P1 123.4(2) . . ?
N2 N1 P1 117.6(2) . . ?
N2 N1 C1 118.9(3) . . ?
C3 N4 C5 106.6(3) . . ?
C3 N4 C6 127.5(3) . . ?
C5 N4 C6 125.9(3) . . ?
C3 N3 Co1 114.3(2) . . ?
C3 N3 C4 105.5(3) . . ?
C4 N3 Co1 140.0(2) . . ?
N4 C3 C2 127.9(3) . . ?
N3 C3 N4 111.6(3) . . ?
N3 C3 C2 120.5(3) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 N2 Co1 124.9(2) . . ?
C2 N2 Co1 114.9(2) . . ?
C2 N2 N1 119.7(3) . . ?
C3 C2 H2 123.0 . . ?
N2 C2 C3 114.1(3) . . ?
N2 C2 H2 123.0 . . ?
N3 C4 H4 125.3 . . ?
C5 C4 N3 109.4(3) . . ?
C5 C4 H4 125.3 . . ?
N4 C5 H5 126.6 . . ?
C4 C5 N4 106.9(3) . . ?
C4 C5 H5 126.6 . . ?
N4 C6 H6A 109.5 . . ?
N4 C6 H6B 109.5 . . ?
N4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O2 Cl1 O2 110.54(16) 3_645 5_765 ?
O2 Cl1 O2 110.54(16) 5_765 . ?
O2 Cl1 O2 110.53(16) 3_645 . ?
O1 Cl1 O2 108.39(16) . . ?
O1 Cl1 O2 108.38(16) . 3_645 ?
O1 Cl1 O2 108.38(16) . 5_765 ?
O3 Cl2 O4 111.6(4) . 3_545 ?
O3 Cl2 O4 111.6(4) . . ?
O3 Cl2 O4 111.6(4) . 5_655 ?
O4A Cl2 O3A 112.3(3) . 5_655 ?
O4A Cl2 O3A 112.3(3) . . ?
O4A Cl2 O3A 112.3(3) . 3_545 ?
O3A Cl2 O3A 106.5(3) 5_655 . ?
O3A Cl2 O3A 106.5(3) 3_545 . ?
O3A Cl2 O3A 106.5(3) 3_545 5_655 ?
O4 Cl2 O4 107.3(4) . 5_655 ?
O4 Cl2 O4 107.3(4) 3_545 5_655 ?
O4 Cl2 O4 107.3(4) . 3_545 ?
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
Co1 N3 2.098(3) . ?
Co1 N3 2.098(3) 3_655 ?
Co1 N3 2.098(3) 5_665 ?
Co1 N2 2.225(3) . ?
Co1 N2 2.225(3) 5_665 ?
Co1 N2 2.225(3) 3_655 ?
S1 P1 1.917(2) . ?
P1 N1 1.686(3) 3_655 ?
P1 N1 1.686(3) . ?
P1 N1 1.686(3) 5_665 ?
N1 C1 1.461(4) . ?
N1 N2 1.375(4) . ?
N4 C3 1.350(4) . ?
N4 C5 1.376(5) . ?
N4 C6 1.466(4) . ?
N3 C3 1.333(4) . ?
N3 C4 1.376(4) . ?
C3 C2 1.450(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
N2 C2 1.293(4) . ?
C2 H2 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.363(5) . ?
C5 H5 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Cl1 O2 1.444(3) 5_765 ?
Cl1 O2 1.444(3) . ?
Cl1 O2 1.444(3) 3_645 ?
Cl1 O1 1.437(5) . ?
Cl2 O3 1.348(14) . ?
Cl2 O4A 1.338(18) . ?
Cl2 O3A 1.479(7) 5_655 ?
Cl2 O3A 1.479(7) 3_545 ?
Cl2 O3A 1.479(7) . ?
Cl2 O4 1.456(10) 5_655 ?
Cl2 O4 1.456(10) . ?
Cl2 O4 1.456(10) 3_545 ?
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
Co1 N3 C3 N4 -177.5(2) . . . . ?
Co1 N3 C3 C2 3.3(4) . . . . ?
Co1 N3 C4 C5 175.7(3) . . . . ?
Co1 N2 C2 C3 -6.9(4) . . . . ?
S1 P1 N1 C1 -10.8(3) . . . . ?
S1 P1 N1 N2 172.90(19) . . . . ?
P1 N1 N2 Co1 12.5(3) . . . . ?
P1 N1 N2 C2 -175.9(2) . . . . ?
N1 P1 N1 C1 112.9(3) 5_665 . . . ?
N1 P1 N1 C1 -134.5(3) 3_655 . . . ?
N1 P1 N1 N2 -63.4(2) 5_665 . . . ?
N1 P1 N1 N2 49.2(2) 3_655 . . . ?
N1 N2 C2 C3 -179.3(3) . . . . ?
N4 C3 C2 N2 -176.4(3) . . . . ?
N3 C3 C2 N2 2.7(4) . . . . ?
N3 C4 C5 N4 0.2(4) . . . . ?
C3 N4 C5 C4 -0.7(4) . . . . ?
C3 N3 C4 C5 0.4(4) . . . . ?
C1 N1 N2 Co1 -164.0(2) . . . . ?
C1 N1 N2 C2 7.6(4) . . . . ?
C4 N3 C3 N4 -0.8(4) . . . . ?
C4 N3 C3 C2 179.9(3) . . . . ?
C5 N4 C3 N3 1.0(4) . . . . ?
C5 N4 C3 C2 -179.9(3) . . . . ?
C6 N4 C3 N3 179.9(3) . . . . ?
C6 N4 C3 C2 -0.9(6) . . . . ?
C6 N4 C5 C4 -179.7(3) . . . . ?
