Effects of coordination sphere on unusually large zero field splitting and slow magnetic relaxation in trigonally symmetric molecules.
Schulte, Kelsey A.; Vignesh, Kuduva R.; Dunbar, Kim R.; Chemical science 9 (2018) 9018–9026; doi:10.1039/c8sc02820f

data_1549971
_publ_section_title
;
 Effects of coordination sphere on unusually large zero field splitting
 and slow magnetic relaxation in trigonally symmetric molecules.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              9018
_journal_page_last               9026
_journal_paper_doi               10.1039/c8sc02820f
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C33 H47 Co N4 O7 S3, C H2 Cl2, H2 O, C4 H12 N'
_chemical_formula_sum            'C38 H63 Cl2 Co N5 O8 S3'
_chemical_formula_weight         943.94
_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   mixed
_audit_creation_date             2018-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-22 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                107.139(2)
_cell_angle_beta                 97.232(2)
_cell_angle_gamma                101.356(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8767(7)
_cell_length_b                   14.5893(11)
_cell_length_c                   19.0022(14)
_cell_measurement_reflns_used    20240
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.79
_cell_measurement_theta_min      4.71
_cell_volume                     2260.7(3)
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26923
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.031
_diffrn_reflns_theta_min         2.481
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.799
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1305 before and 0.0582 after correction. The Ratio of minimum to maximum transmission is 0.6746. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.282
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         7962
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+4.8812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7577
_reflns_number_total             7962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02820f2.cif
_cod_data_source_block           co_mst_oh2
_cod_depositor_comments
'Adding full bibliography for 1549971--1549976.cif.'
_cod_database_code               1549971
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.292
_shelx_estimated_absorpt_t_min   0.223
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Cl2A-C38A \\sim Cl1-C38 \\sim Cl2-C38 \\sim Cl1A-C38A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl2A \\sim Cl1A \\sim Cl1 \\sim C38A \\sim C38 \\sim Cl2: within 1.9A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Cl2A)=Sof(Cl1A)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C38)=Sof(H38A)=Sof(H38B)=FVAR(1)
5.a Free rotating group:
 O8(H8D,H8E)
5.b Rotating group:
 O7(H7A,H7B)
5.c Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C1(H1A,H1B), C2(H2A,H2B), C12(H12A,H12B),
 C13(H13A,H13B), C38(H38A,H38B), C38A(H38C,H38D)
5.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C6(H6), C17(H17), C31(H31), C28(H28), C20(H20)
5.e Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C33(H33A,H33B,H33C), C16(H16A,H16B,H16C), C11(H11A,H11B,
 H11C), C27(H27A,H27B,H27C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C35(H35A,
 H35B,H35C), C8(H8A,H8B,H8C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C),
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'