Generation and characterisation of a stable nickel(II)-aminoxyl radical complex
Parrot, Arnaud; Yuma, Morimoto; Paria, Sayantan; Sugimoto, Hideki; Fujieda, Nobutaka; Itoh, Shinobu; Dalton Trans.  (2017) –; doi:10.1039/C7DT01789H

data_7043183
_publ_section_title
;
 Generation and characterisation of a stable nickel(II)-aminoxyl radical
 complex
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01789H
_journal_year                    2017
_chemical_formula_moiety         'C105 H144 N6 Ni O9'
_chemical_formula_sum            'C105 H144 N6 Ni O9'
_chemical_formula_weight         1693.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-01-26 deposited with the CCDC.
2017-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.4711(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   28.9848(13)
_cell_length_b                   24.5064(13)
_cell_length_c                   28.3120(12)
_cell_measurement_reflns_used    40569
_cell_measurement_temperature    103
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.00
_cell_volume                     20018.8(16)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.2'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1948
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            97719
_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         27.483
_diffrn_reflns_theta_min         3.000
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7328.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.70
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         22924
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.2080
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1017P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.2395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9266
_reflns_number_total             22924
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7dt01789h2.cif
_cod_data_source_block           130612
_cod_database_code               7043183
_shelx_res_checksum              53417