Synthesis, Structure, and Magnetism of Mono- and Binuclear Manganese(II) Compounds of Nitronyl Nitroxide Substituted Phosphine Oxides
Corinne Rancurel; Daniel B. Leznoff; Jean-Pascal Sutter; Stéphane Golhen; Lahcène Ouahab; Janis Kliava; Olivier Kahn; Inorganic Chemistry 38 (1999) 4753–4758; doi:10.1021/ic990527g

data_4322319
_publ_section_title
;
 Synthesis, Structure, and Magnetism of Mono- and Binuclear Manganese(II)
 Compounds of Nitronyl Nitroxide Substituted Phosphine Oxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4753
_journal_page_last               4758
_journal_paper_doi               10.1021/ic990527g
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C70 H56 F24 Mn2 N4 O14 P2'
_chemical_formula_weight         1805.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 98.49(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.463(6)
_cell_length_b                   19.315(3)
_cell_length_c                   17.084(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.930
_cell_measurement_theta_min      5.240
_cell_volume                     4067(3)
_computing_cell_refinement       'Nonius CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        MolEN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       q\2q
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8346
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        0.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.999837
_exptl_absorpt_correction_T_min  0.983021
_exptl_absorpt_correction_type   '\y scan'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7961
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1706
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1089P)^2^+2.1057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.2213
_reflns_number_gt                3936
_reflns_number_total             7961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990527g_2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1089P)^2^+2.1057P] 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^)+(0.1089P)^2^+2.1057P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322319