Structures of Bisphosphonate Metal Complexes: Zinc and Cadmium Complexes of Clodronate and Its Partial Ester Derivatives
Mervi Kontturi; Elina Laurila; Riikka Mattsson; Sirpa Peräniemi; Jouko J. Vepsäläinen; Markku Ahlgrén; Inorganic Chemistry 44 (2005) 2400–2406; doi:10.1021/ic048329z

data_4308954
_publ_contact_author_address
;
        Department of Chemistry
        University of Joensuu
        P.O. Box 111
        FI-80101, Joensuu
        Finland
;
_publ_contact_author_email       mervi.kontturi@joensuu.fi
_publ_contact_author_fax         '358 13 2513390'
_publ_contact_author_name        'Mervi Kontturi'
_publ_contact_author_phone       '358 13 2513377'
_publ_section_title
;
Structures of Bisphosphonate Metal Complexes: Zinc and Cadmium Complexes
of Clodronate and Its Partial Ester Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2400
_journal_page_last               2406
_journal_paper_doi               10.1021/ic048329z
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C32 H80 Cd4 Cl8 O32 P8, 2(H2 O)'
_chemical_formula_sum            'C32 H84 Cd4 Cl8 O34 P8'
_chemical_formula_weight         1993.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.1647(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9504(2)
_cell_length_b                   12.3418(2)
_cell_length_c                   21.0920(2)
_cell_measurement_reflns_used    54179
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.91
_cell_volume                     3621.88(9)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'collect (Nonius BV, 1997 - 2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL v.5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       CCD
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54179
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  0.7836
_exptl_absorpt_correction_T_min  0.7836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP in SHELXTL v.5.1 (Bruker AXS, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      1.79(2)
_exptl_crystal_density_method    'flotation in cyclohexane/bromoform'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.587
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00096(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   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                6391
_reflns_number_total             7102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048329zsi20050201_035527_1.cif
_cod_data_source_block           Structure4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4308954