Synthesis and Characterization of the Open-Framework Barium Bisphosphonate [Ba3(O3PCH2NH2CH2PO3)2(H2O)4]·3H2O
Bauer, Sebastian; Müller, Helen; Bein, Thomas; Stock, Norbert; Inorganic Chemistry 44 (2005) 9464–9470; doi:10.1021/ic050935m

data_4331544
_publ_section_title
;
 Synthesis and Characterization of the Open-Framework Barium
 Bisphosphonate [Ba3(O3PCH2NH2CH2PO3)2(H2O)4]&#x00B7;3H2O
;
_journal_issue                   25
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9464
_journal_page_last               9470
_journal_paper_doi               10.1021/ic050935m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C4 H32 Ba3 N2 O19 P4'
_chemical_formula_weight         948.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.732(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.287(2)
_cell_length_b                   13.5995(7)
_cell_length_c                   7.1862(6)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      3.0
_cell_volume                     2249.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(3)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'area detection'
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9531
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         3.00
_diffrn_source_current           50
_diffrn_source_power             2.75
_diffrn_source_voltage           55
_exptl_absorpt_coefficient_mu    5.568
_exptl_absorpt_correction_T_max  0.8471
_exptl_absorpt_correction_T_min  0.4577
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.652
_refine_diff_density_min         -1.765
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.00038(6)
_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   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0320P)^2^+18.6310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                2298
_reflns_number_total             2677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050935msup1.cif
_cod_data_source_block           Ba3[O3PCH2NH2PO3]2_13H2O
_cod_original_cell_volume        2249.5(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4331544