#------------------------------------------------------------------------------
#$Date: 2017-03-04 15:25:45 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193460 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/50/4345036.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_4345036
loop_
_publ_author_name
'Shao, Feng'
'Cahier, Benjamin'
'Rivière, Eric'
'Guillot, Régis'
'Guihéry, Nathalie'
'Campbell, Victoria E.'
'Mallah, Talal'
_publ_section_title
;
 Structural Dependence of the Ising-type Magnetic Anisotropy and of the
 Relaxation Time in Mononuclear Trigonal Bipyramidal Co(II) Single
 Molecule Magnets.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1104
_journal_page_last               1111
_journal_paper_doi               10.1021/acs.inorgchem.6b01966
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H39 Co N2 S4, Cl O4'
_chemical_formula_sum            'C19 H39 Cl Co N2 O4 S4'
_chemical_formula_weight         582.14
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      198
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1508(5)
_cell_length_b                   14.1508(5)
_cell_length_c                   14.1508(5)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.49
_cell_volume                     2833.63(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43924
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.564
_diffrn_reflns_theta_min         2.035
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_correction_T_min  0.8951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 1135 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.050(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0468P)²+5.9343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2737
_reflns_number_total             2921
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01966_si_004.cif
_cod_data_source_block           3
_cod_depositor_comments          'Adding full bibliography for 4345036.cif.'
_cod_original_cell_volume        2833.6(3)
_cod_database_code               4345036
_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   0.954
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+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
C00C C 0.5610(4) 0.0610(4) 0.4390(4) 0.0253(17) Uani 1 3 d S T P
C1 C 0.7738(4) 0.3848(3) 0.2435(3) 0.0263(10) Uani 1 1 d . . .
H1A H 0.7156 0.4108 0.2147 0.032 Uiso 1 1 calc R U .
H1B H 0.8282 0.4209 0.2183 0.032 Uiso 1 1 calc R U .
C2 C 0.7692(5) 0.3974(4) 0.3495(4) 0.0336(12) Uani 1 1 d . . .
H2A H 0.7646 0.4653 0.3656 0.040 Uiso 1 1 calc R U .
H2B H 0.8267 0.3713 0.3795 0.040 Uiso 1 1 calc R U .
C3 C 0.6835(4) 0.3279(3) 0.5204(3) 0.0276(10) Uani 1 1 d . . .
C4 C 0.7624(5) 0.2590(5) 0.5451(4) 0.0362(13) Uani 1 1 d . . .
H4A H 0.8208 0.2785 0.5135 0.054 Uiso 1 1 calc R U .
H4B H 0.7449 0.1954 0.5239 0.054 Uiso 1 1 calc R U .
H4C H 0.7722 0.2586 0.6136 0.054 Uiso 1 1 calc R U .
C5 C 0.7047(6) 0.4268(4) 0.5569(4) 0.0487(19) Uani 1 1 d . . .
H5A H 0.6569 0.4709 0.5332 0.073 Uiso 1 1 calc R U .
H5B H 0.7673 0.4465 0.5347 0.073 Uiso 1 1 calc R U .
H5C H 0.7037 0.4265 0.6261 0.073 Uiso 1 1 calc R U .
C6 C 0.5883(4) 0.2929(4) 0.5593(4) 0.0339(13) Uani 1 1 d . . .
H6A H 0.5926 0.2861 0.6281 0.051 Uiso 1 1 calc R U .
H6B H 0.5729 0.2316 0.5309 0.051 Uiso 1 1 calc R U .
H6C H 0.5387 0.3387 0.5436 0.051 Uiso 1 1 calc R U .
N1 N 0.7837(2) 0.2837(2) 0.2163(2) 0.0126(11) Uani 1 3 d S T P
N2 N 0.6064(3) 0.1064(3) 0.3936(3) 0.0175(12) Uani 1 3 d S T P
O1 O 0.7835(2) 0.7165(2) 0.2835(2) 0.0292(14) Uani 1 3 d S T P
O2 O 0.7861(2) 0.6199(3) 0.4182(2) 0.0239(7) Uani 1 1 d . . .
S1 S 0.66536(9) 0.33500(8) 0.39059(8) 0.0229(3) Uani 1 1 d . . .
S2 S 0.49472(12) -0.00528(12) 0.50528(12) 0.0627(11) Uani 1 3 d S T P
Cl1 Cl 0.84227(7) 0.65773(7) 0.34227(7) 0.0154(3) Uani 1 3 d S T P
Co1 Co 0.68801(4) 0.18801(4) 0.31199(4) 0.01020(19) Uani 1 3 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1250 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3490 0.9758 '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
N2 C00C S2 180.0(13) . .
N1 C1 C2 112.0(4) . .
N1 C1 H1A 109.2 . .
C2 C1 H1A 109.2 . .
N1 C1 H1B 109.2 . .
C2 C1 H1B 109.2 . .
H1A C1 H1B 107.9 . .
C1 C2 S1 107.2(4) . .
C1 C2 H2A 110.3 . .
S1 C2 H2A 110.3 . .
C1 C2 H2B 110.3 . .
S1 C2 H2B 110.3 . .
H2A C2 H2B 108.5 . .
C5 C3 C4 111.5(6) . .
C5 C3 C6 110.4(5) . .
C4 C3 C6 110.7(5) . .
C5 C3 S1 108.2(4) . .
C4 C3 S1 111.2(3) . .
C6 C3 S1 104.5(4) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C3 C6 H6A 109.5 . .
C3 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C3 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C1 N1 C1 108.4(3) . 8_645
C1 N1 C1 108.4(3) . 11_556
C1 N1 C1 108.4(3) 8_645 11_556
C1 N1 Co1 110.5(3) . .
C1 N1 Co1 110.5(3) 8_645 .
C1 N1 Co1 110.5(3) 11_556 .
C00C N2 Co1 180.0(8) . .
C2 S1 C3 103.4(3) . .
C2 S1 Co1 99.61(18) . .
C3 S1 Co1 113.36(16) . .
O2 Cl1 O2 109.89(16) . 6_566
O2 Cl1 O2 109.89(16) . 12_664
O2 Cl1 O2 109.89(16) 6_566 12_664
O2 Cl1 O1 109.04(16) . .
O2 Cl1 O1 109.05(16) 6_566 .
O2 Cl1 O1 109.05(16) 12_664 .
N2 Co1 N1 180.00(12) . .
N2 Co1 S1 99.03(4) . .
N1 Co1 S1 80.97(4) . .
N2 Co1 S1 99.03(4) . 8_645
N1 Co1 S1 80.97(4) . 8_645
S1 Co1 S1 117.582(18) . 8_645
N2 Co1 S1 99.03(4) . 11_556
N1 Co1 S1 80.97(4) . 11_556
S1 Co1 S1 117.583(18) . 11_556
S1 Co1 S1 117.582(18) 8_645 11_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C00C N2 1.112(12) .
C00C S2 1.625(10) .
C1 N1 1.488(5) .
C1 C2 1.512(7) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 S1 1.810(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C5 1.520(7) .
C3 C4 1.524(9) .
C3 C6 1.536(8) .
C3 S1 1.858(5) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
N1 C1 1.488(5) 8_645
N1 C1 1.488(5) 11_556
N1 Co1 2.346(6) .
N2 Co1 2.001(7) .
O1 Cl1 1.440(6) .
O2 Cl1 1.439(3) .
S1 Co1 2.3804(11) .
Cl1 O2 1.439(3) 6_566
Cl1 O2 1.439(3) 12_664
Co1 S1 2.3804(11) 8_645
Co1 S1 2.3804(11) 11_556
