Structural Variations within Group 1 (Li-Cs)+(2,2,6,6-Tetramethyl-1-piperidinyloxy)-Complexes Made via Metallic Reduction of the Nitroxyl Radical
Liam Balloch; Allison M. Drummond; Pablo García-Álvarez; David V. Graham; Alan R. Kennedy; Jan Klett; Robert E. Mulvey; Charles T. O'Hara; Philip J. A. Rodger; Iain D. Rushworth; Inorganic Chemistry 48 (2009) 6934–6944; doi:10.1021/ic900609e

data_4302684
_publ_section_title
;
Structural Variations within Group 1
(Li-Cs)+(2,2,6,6-Tetramethyl-1-piperidinyloxy)-Complexes Made via
Metallic Reduction of the Nitroxyl Radical
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6934
_journal_page_last               6944
_journal_paper_doi               10.1021/ic900609e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C48 H104 N8 Na4 O4'
_chemical_formula_weight         949.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.066(2)
_cell_angle_beta                 90.989(3)
_cell_angle_gamma                112.001(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5872(4)
_cell_length_b                   12.6456(4)
_cell_length_c                   20.7262(4)
_cell_measurement_reflns_used    19114
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.3167
_cell_measurement_theta_min      2.5988
_cell_volume                     2815.28(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            52741
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       FRAGMENT
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         13559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.0342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                9567
_reflns_number_total             13559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900609e_si_001_4.cif
_cod_data_source_block           pgaliam2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2815.28(14)
_cod_database_code               4302684