An indication of spin-transition accompanied by an order-disorder structural transformation in [Ni(phpyNO)2(NCS)2] (phpyNO = tert-butyl 5-phenyl-2-pyridyl nitroxide)
Kyoden, Yukiya; Ishida, Takayuki; RSC Advances 10 (2020) 16009–16015; doi:10.1039/D0RA02041A

data_7240393
_publ_section_title
;
 An indication of spin-transition accompanied by an order-disorder
 structural transformation in [Ni(phpyNO)2(NCS)2] (phpyNO = tert-butyl
 5-phenyl-2-pyridyl nitroxide)
;
_journal_issue                   27
_journal_name_full               'RSC Advances'
_journal_page_first              16009
_journal_page_last               16015
_journal_paper_doi               10.1039/D0RA02041A
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C32 H34 N6 Ni O2 S2'
_chemical_formula_sum            'C32 H34 N6 Ni O2 S2'
_chemical_formula_weight         657.48
_chemical_name_systematic        '[Ni(phpyNO)2(NCS)2]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc24lhpy
_audit_update_record
;
2020-02-14 deposited with the CCDC.	2020-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   17.0732(19)
_cell_length_b                   19.194(3)
_cell_length_c                   20.667(3)
_cell_measurement_reflns_used    25622
_cell_measurement_temperature    400
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.10
_cell_volume                     6772.6(16)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'CrystalStructure 4.2.1'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus, et al., 2007)'
_diffrn_ambient_temperature      400
_diffrn_detector_area_resol_mean 29.412
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1293
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            75566
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.596
_diffrn_reflns_theta_min         3.095
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2752.00
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.177
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7078
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1954
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0514P)^2^+2.6054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3016
_reflns_number_total             7078
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d0ra02041a1.cif
_cod_data_source_block           phpyNO_Ni_NCS2_400K
_cod_depositor_comments
'Adding full bibliography for 7240392--7240393.cif.'
_cod_original_cell_volume        6772.7(16)
_cod_database_code               7240393
_shelx_res_checksum              63108