Tris(nitrato-κ^2^<i>O</i>,<i>O</i>')bis[4,4,5,5-tetramethyl-2-(pyridin-2-yl-κ<i>N</i>)imidazoline-1-oxyl 3-oxide-κ<i>O</i>]holmium(III)
Li, Dong-Jiao; Acta Crystallographica Section E 68 (2012) m550–; doi:10.1107/S1600536812012445

data_2234684
_publ_section_title
;
 Tris(nitrato-\k^2^<i>O</i>,<i>O</i>')bis[4,4,5,5-tetramethyl-2-(pyridin-2-yl-\k<i>N</i>)imidazoline-1-oxyl
 3-oxide-\k<i>O</i>]holmium(III)
;
_journal_coeditor_code           IS5078
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m550
_journal_paper_doi               10.1107/S1600536812012445
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ho (N O3)3 (C12 H16 N3 O2)2]'
_chemical_formula_moiety         'C24 H32 Ho N9 O13'
_chemical_formula_sum            'C24 H32 Ho N9 O13'
_chemical_formula_weight         819.52
_chemical_name_systematic
;
Tris(nitrato-\k^2^<i>O</i>,<i>O</i>')bis[4,4,5,5-tetramethyl-2-(pyridin-
2-yl-\k<i>N</i>)imidazoline-1-oxyl 3-oxide-\k<i>O</i>]holmium(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.391(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2627(10)
_cell_length_b                   11.1044(8)
_cell_length_c                   23.2861(17)
_cell_measurement_reflns_used    2811
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7933
_cell_measurement_theta_min      2.5105
_cell_volume                     3136.9(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17689
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.19
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.601
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.866
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                4895
_reflns_number_total             5530
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is5078.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2234684
_cod_database_fobs_code          2234684