New Types of Metal Squarato-phosphonates: Condensation of Aminodiphosphonate with Squaric Acid under Hydrothermal Conditions
Bing-Ping Yang; Jiang-Gao Mao; Inorganic Chemistry 44 (2005) 566–571; doi:10.1021/ic048685h

data_4308457
_publ_contact_author_address
;
     Fujian Institute of Research  
        on the Structure of Matter,
        Chinese Academy of Sciences,
        Fuzhou, Fujian 350002, 
    P.R.China
;
_publ_contact_author_email       mjg@ms.fjirsm.ac.cn
_publ_contact_author_fax         0086-0591-3704836
_publ_contact_author_name        'Dr. Jiang-Gao Mao'
_publ_contact_author_phone       0086-0591-3704836
_publ_section_title
;
New Types of Metal Squarato-phosphonates: Condensation of
Aminodiphosphonate with Squaric Acid under Hydrothermal Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              566
_journal_page_last               571
_journal_paper_doi               10.1021/ic048685h
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C12 H32 Mn3 N2 O28 P4'
_chemical_formula_sum            'C12 H32 Mn3 N2 O28 P4'
_chemical_formula_weight         941.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.724(2)
_cell_angle_beta                 103.905(2)
_cell_angle_gamma                90.657(2)
_cell_formula_units_Z            1
_cell_length_a                   7.62670(10)
_cell_length_b                   8.16890(10)
_cell_length_c                   12.8587(4)
_cell_measurement_reflns_used    2684
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.64
_cell_volume                     773.24(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Siemens 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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4049
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67621
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             477
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0507P)^2^+7.9220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                2169
_reflns_number_total             2684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048685hsi20040920_050335.cif
_cod_data_source_block           Mn
_cod_database_code               4308457