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_4339255
_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 H88 N8 Ni2 O34.625 P2'
_chemical_formula_weight         1510.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :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            32
_cell_length_a                   42.9658(7)
_cell_length_b                   42.9658(7)
_cell_length_c                   29.3862(9)
_cell_measurement_reflns_used    5074
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      15.30
_cell_measurement_theta_min      2.33
_cell_volume                     54249(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1652
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            171529
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             25440
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.685
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         8880
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.1063
_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^)+(0.1759P)^2^+730.6161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2784
_refine_ls_wR_factor_ref         0.3496
_reflns_number_gt                5312
_reflns_number_total             8880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700439a.cif
_cod_data_source_block           i41acd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/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 
;
_cod_original_sg_symbol_H-M      I4(1)/acd
_cod_database_code               4339255