The tetramethylpiperidinyl-1-oxide anion (TMPO‒) as a ligand in lanthanide chemistry: synthesis of the per(TMPO‒) complex [(ONC5H6Me4)2Sm( µ-ONC5H6Me4)]2
Evans, William J.; Perotti, Jeremy M.; Doedens, Robert J.; Ziller, Joseph W.; Chemical Communications  (2001) 2326–; doi:10.1039/b106869p

data_7114708
_publ_section_title
;
 The tetramethylpiperidinyl-1-oxide anion (TMPO--) as a ligand in
 lanthanide chemistry: synthesis of the per(TMPO--) complex
 [(ONC5H6Me4)2Sm( &#x00B5;-ONC5H6Me4)]2
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2326
_journal_paper_doi               10.1039/b106869p
_journal_year                    2001
_chemical_formula_sum            'C38 H66 Cl2 N2 O2 Sm2'
_chemical_formula_weight         954.53
_chemical_name_systematic
; 
? 
;
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 106.306(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.5950(19)
_cell_length_b                   8.3464(11)
_cell_length_c                   17.584(2)
_cell_measurement_temperature    163(2)
_cell_volume                     2055.8(4)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20947
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        '< 1.0'
_exptl_absorpt_coefficient_mu    2.990
_exptl_absorpt_correction_T_max  0.8180
_exptl_absorpt_correction_T_min  0.5463
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         5015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0250P)^2^+3.7826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                3567
_reflns_number_total             5015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106869p.txt
_cod_data_source_block           jp3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2055.9(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114708