Syntheses, structures, magnetic, and spectroscopic properties of cobalt(ii), nickel(ii) and zinc(ii) complexes containing 2-(6-methyl)pyridyl-substituted nitronyl and imino nitroxide†
Yamamoto, Youhei; Suzuki, Takayoshi; Kaizaki, Sumio; Journal of the Chemical Society, Dalton Transactions  (2001) 2943–; doi:10.1039/b103647p

data_7702616
_publ_section_title
;
 Syntheses, structures, magnetic, and spectroscopic properties of
 cobalt(ii), nickel(ii) and zinc(ii) complexes containing
 2-(6-methyl)pyridyl-substituted nitronyl and imino nitroxide&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2943
_journal_paper_doi               10.1039/b103647p
_journal_year                    2001
_chemical_formula_moiety         '(Co Br2 (C13 H18 N3 O2))'
_chemical_formula_sum            'C13 H18 Br2 Co N3 O2'
_chemical_formula_weight         467.05
_chemical_name_common            '[CoBr~2~(NITmepy)]'
_chemical_name_systematic
;
Dibromo(2-(2-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide)cobalt(I
I)
;
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.491(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3499(18)
_cell_length_b                   19.4867(15)
_cell_length_c                   12.055(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     1718.7(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_sigmaI/netI    0.0899
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5371
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        1.72
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.654
_exptl_absorpt_correction_T_max  0.464
_exptl_absorpt_correction_T_min  0.235
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            darkpurple
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                2676
_reflns_number_total             5371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b103647p.txt
_cod_data_source_block           CoBrNIT
_cod_original_cell_volume        1718.6(5)
_cod_database_code               7702616