Complex chemistry of 2,2,6,6-tetramethyl-4-(2,2′∶6′,2″-terpyridin-4′-yloxy)piperidin-1-oxyl, a spin-labelled terpyridine ‡
Halcrow, Malcolm A.; Brechin, Euan K.; McInnes, Eric J. L.; Mabbs, Frank E.; Davies, John E.; Journal of the Chemical Society, Dalton Transactions  (1998) 2477–; doi:10.1039/a803793k

data_7028198
_publ_section_title
;
 Complex chemistry of
 2,2,6,6-tetramethyl-4-(2,2&#x2032;&#x2236;6&#x2032;,2&#x2033;-terpyridin-4&#x2032;-yloxy)piperidin-1-oxyl,
 a spin-labelled terpyridine&#x200A;&#x2021;
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2477
_journal_paper_doi               10.1039/a803793k
_journal_year                    1998
_chemical_formula_sum            'C51 H58.5 B2 F8 Mn N9.5 O4.25'
_chemical_formula_weight         1101.13
_chemical_name_systematic
;

Bis-[4-(2,2':6',2''-terpyrid-4'-yloxy)-2,2,6,6-tetramethyl-1-piperidinoxyl]

manganese(II) ditetrafluoroborate acetonitrile solvate.

;
_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
_cell_angle_alpha                90.68(2)
_cell_angle_beta                 93.29(2)
_cell_angle_gamma                114.110(10)
_cell_formula_units_Z            2
_cell_length_a                   17.403(3)
_cell_length_b                   18.906(4)
_cell_length_c                   9.077(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     2719.5(10)
_computing_cell_refinement       'Rigaku control software'
_computing_data_collection       'Rigaku control software'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1995)'
_computing_molecular_graphics    'Siemens SHELXTL (Sheldrick, 1987)'
_computing_publication_material  'Siemens SHELXTL (Sheldrick, 1987)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       'omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8834
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        3.2%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         8514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_obs          0.0640
_refine_ls_shift/esd_max         -0.036
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+3.2596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1912
_refine_ls_wR_factor_obs         0.1690
_reflns_number_observed          6266
_reflns_number_total             8514
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            k803793sup1.cif
_cod_data_source_block           mh288/mh9602
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+3.2596P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+3.2596P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C51 H58.50 B2 F8 Mn N9.50 O4.25'
_cod_database_code               7028198