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_1549974
_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 N4 Ni O7 S3, C4 H12 N, H2 O, 0.5(C4 H10 O)'
_chemical_formula_sum            'C39 H66 N5 Ni O8.5 S3'
_chemical_formula_weight         895.85
_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                107.6400(10)
_cell_angle_beta                 99.2520(10)
_cell_angle_gamma                103.1570(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9571(7)
_cell_length_b                   14.5969(11)
_cell_length_c                   18.6587(14)
_cell_measurement_reflns_used    27420
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.48
_cell_measurement_theta_min      2.56
_cell_volume                     2193.3(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    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  Venture
_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  0.0206
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33212
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.478
_diffrn_reflns_theta_min         2.565
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.432
_exptl_absorpt_correction_T_max  0.8256
_exptl_absorpt_correction_T_min  0.6173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1240 before and 0.0355 after correction. The Ratio of minimum to maximum transmission is 0.7477. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         8549
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0396P)^2^+1.4536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8191
_reflns_number_total             8549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02820f2.cif
_cod_data_source_block           ni_mst_oh2
_cod_depositor_comments
'Adding full bibliography for 1549971--1549976.cif.'
_cod_original_formula_sum        'C39 H66 N5 Ni O8.50 S3'
_cod_database_code               1549974
_shelx_shelxl_version_number     2014/7
_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
 N5-C35 \\sim N5-C35A \\sim N5-C36 \\sim N5-C36A \\sim N5-C37 \\sim N5-C37A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C35 \\sim C35A \\sim C36 \\sim C36A \\sim C37A \\sim C37 \\sim N5: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
 Fixed Sof: O9(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C39(0.5) H39A(0.5)
 H39B(0.5) C40(0.5) H40A(0.5) H40B(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5)
5.a Free rotating group:
 O8(H8D,H8E)
5.b Rotating group:
 O7(H7A,H7B)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C23(H23A,H23B), C12(H12A,H12B), C1(H1A,H1B), C24(H24A,H24B),
 C13(H13A,H13B), C39(H39A,H39B), C40(H40A,H40B)
5.d Aromatic/amide H refined with riding coordinates:
 C17(H17), C31(H31), C20(H20), C28(H28), C6(H6), C9(H9)
5.e Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C5(H5A,H5B,
 H5C), C11(H11A,H11B,H11C), C33(H33A,H33B,H33C), C27(H27A,H27B,H27C), C8(H8A,
 H8B,H8C), C19(H19A,H19B,H19C), C30(H30A,H30B,H30C), C36(H36A,H36B,H36C),
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C41(H41A,H41B,
 H41C), C35A(H35D,H35E,H35F), C36A(H36D,H36E,H36F), C37A(H37D,H37E,H37F)
;
_olex2_submission_special_instructions 'No special instructions were received'