DOTP-Manganese and -Nickel Complexes: from a Tetrahedral Network with 12-Membered Rings to an Ionic Phosphonate
Kong; Dmitri G. Medvedev; Abraham Clearfield; Inorganic Chemistry 43 (2004) 7308–7314; doi:10.1021/ic040076m

data_4311974
_publ_section_title
;
 DOTP-Manganese and -Nickel Complexes: from a Tetrahedral Network with
 12-Membered Rings to an Ionic Phosphonate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7308
_journal_page_last               7314
_journal_paper_doi               10.1021/ic040076m
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C12 H32 Mn N4 O12 P4'
_chemical_formula_weight         603.24
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.349(2)
_cell_length_b                   12.349(2)
_cell_length_c                   14.066(4)
_cell_measurement_temperature    383(2)
_cell_volume                     2145.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      383(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0116
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8412
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    0.986
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1252
_refine_diff_density_max         2.277
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0018(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          1.261
_refine_ls_shift/su_mean         0.110
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+5.9660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                759
_reflns_number_total             776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040076m_2.cif
_cod_data_source_block           sol
_cod_original_cell_volume        2144.9(8)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4311974