Magnetism behaviours dominated by the interplay of magnetic anisotropy and exchange coupling in local Co discs.
Yang, En-Cui; Liu, Zhong-Yi; Zhang, Lei; Yang, Na; Zhao, Xiao-Jun; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8134–8141; doi:10.1039/c6dt00010j

data_7038963
_publ_section_title
;
 Magnetism behaviours dominated by the interplay of magnetic anisotropy
 and exchange coupling in local Co discs.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8134
_journal_page_last               8141
_journal_paper_doi               10.1039/c6dt00010j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '0.5(C52 H56 Co14 N20 O48 S4)'
_chemical_formula_sum            'C26 H28 Co7 N10 O24 S2'
_chemical_formula_weight         1341.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-17 deposited with the CCDC.
2016-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.124(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4315(14)
_cell_length_b                   13.956(3)
_cell_length_c                   20.444(4)
_cell_measurement_reflns_used    496
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.6580
_cell_measurement_theta_min      6.0500
_cell_volume                     2093.5(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -23.00   32.00   1.0000    1.5100
omega____ theta____ kappa____ phi______ frames
    -      -40.1801   38.0000    0.0000 55

  2 omega  -44.00   33.00   1.0000    1.5100
omega____ theta____ kappa____ phi______ frames
    -      -40.1801   38.0000  -60.0000 77

  3 omega  -12.00   34.00   1.0000    1.5100
omega____ theta____ kappa____ phi______ frames
    -      -40.1801   57.0000 -180.0000 46

  4 omega  -60.00  -13.00   1.0000    1.5100
omega____ theta____ kappa____ phi______ frames
    -      -40.1801   57.0000 -180.0000 47

  5 omega   33.00   93.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -45.0000  -60.0000 60

  6 omega   56.00  157.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -15.0000 -150.0000 101

  7 omega   90.00  159.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064   45.0000 -150.0000 69

  8 omega   45.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -45.0000 -120.0000 37

  9 omega   31.00   87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000    0.0000 56

 10 omega   64.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -45.0000   90.0000 33

 11 omega   32.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.5064  -30.0000   60.0000 54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1194437000
_diffrn_orient_matrix_UB_12      0.0693483000
_diffrn_orient_matrix_UB_13      0.0471387000
_diffrn_orient_matrix_UB_21      0.1653594000
_diffrn_orient_matrix_UB_22      -0.0244616000
_diffrn_orient_matrix_UB_23      -0.0339137000
_diffrn_orient_matrix_UB_31      -0.0508092000
_diffrn_orient_matrix_UB_32      0.0822555000
_diffrn_orient_matrix_UB_33      -0.0494229000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.1985
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3444
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.062
_diffrn_reflns_theta_max         67.062
_diffrn_reflns_theta_min         3.851
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.034
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.564
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3444
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.2113
_refine_ls_R_factor_gt           0.1170
_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/[\s^2^(Fo^2^)+(0.1373P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2796
_refine_ls_wR_factor_ref         0.3093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1390
_reflns_number_total             3444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00010j2.cif
_cod_data_source_block           a150427a_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7038962--7038963.cif.'
_cod_original_cell_volume        2093.6(7)
_cod_database_code               7038963
_chemical_oxdiff_formula         'C H O N Zn'
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.512(5) 0.488(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 N6-C6
 1.35 with sigma of 0.01
 N7-C4
 2.3 with sigma of 0.01
 C8-C5
 2.13 with sigma of 0.01
 C8-C4
 2.17 with sigma of 0.01
 N9-N7
 2.33 with sigma of 0.01
 N9-C5
 2.22 with sigma of 0.01
 N7-C5
 1.39 with sigma of 0.01
 C8-N7
 1.37 with sigma of 0.01
 N9-C8
 1.4 with sigma of 0.01
 N9-C4
 1.35 with sigma of 0.01
 C5-C4 = N3-C4 = N3-C2 = N1-C2 = N1-C6 = C6-C5
 1.39 with sigma of 0.01
 N1-N6 \\sim N6-C5
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
N1 \\sim N3 \\sim N6 \\sim N7 \\sim N9 \\sim C2 \\sim C4 \\sim C5 \\sim C6
\\sim C8: within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
C14 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: N6(0.5) H6A(0.5) H6B(0.5) N1(0.5) C2(0.5) H2(0.5) N3(0.5) C4(0.5)
 C5(0.5) N7(0.5) C8(0.5) H8(0.5) N9(0.5) C6(0.5)
6.a Riding coordinates:
 O7W(H7WA,H7WB)
6.b Ternary CH refined with riding coordinates:
 O5(H5), O6(H6)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C2(H2), C8(H8)
6.d Fitted pentagon refined as free rotating group:
 C4(C5,N7,C8,N9)
6.e X=CH2 refined with riding coordinates:
 N6(H6A,H6B)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'