Synthesis and structural and magnetic characterization of {[(phen)(2)Ni](2)(micro-P(2)O(7))} . 27H(2)O and {[(phen)(2)Mn](2)(micro-P(2)O(7))} . 13H(2)O: rare examples of coordination complexes with the pyrophosphate ligand.
Ikotun, Oluwatayo F.; Armatus, N. Gabriel; Julve, Miguel; Kruger, Paul E.; Lloret, Francesc; Nieuwenhuyzen, Mark; Doyle, Robert P.; Inorganic chemistry 46 (2007) 6668–6674; doi:10.1021/ic700439a

data_4339256
_publ_section_title
;
 Synthesis and structural and magnetic characterization of
 {[(phen)(2)Ni](2)(micro-P(2)O(7))} . 27H(2)O and
 {[(phen)(2)Mn](2)(micro-P(2)O(7))} . 13H(2)O: rare examples of
 coordination complexes with the pyrophosphate ligand.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6668
_journal_page_last               6674
_journal_paper_doi               10.1021/ic700439a
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C48 H58 Mn2 N8 O20 P2'
_chemical_formula_weight         1238.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.962(5)
_cell_angle_beta                 77.079(5)
_cell_angle_gamma                82.916(5)
_cell_formula_units_Z            2
_cell_length_a                   13.693(3)
_cell_length_b                   14.093(3)
_cell_length_c                   14.602(3)
_cell_measurement_reflns_used    13434
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      1.43
_cell_volume                     2724.5(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL and Mercury 1.4.1'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'APEX CCD Detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_sigmaI/netI    0.1038
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28966
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.43
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_correction_T_min  0.9419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         13434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0747
_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^)+(0.0782P)^2^+3.6350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1875
_reflns_number_gt                9071
_reflns_number_total             13434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700439a.cif
_cod_data_source_block           p-1
_cod_database_code               4339256