Binary salt of a palladium(II) complex with (phosphonomethyl)phosphonic (medronic) acid comprising `handbell-like' [Pd{μ-CH~2~(PO~3~)~2~}]~3~ units
Babaryk, Artem A.; Kozachkova, Alexandra N.; Tsaryk, Natalia V.; Dudko, Anatolij V.; Pekhnyo, Vasily I.; Acta Crystallographica Section C 68 (2012) m242–m245; doi:10.1107/S0108270112031368

data_2018637
_publ_section_title
;
 Binary salt of a palladium(II) complex with (phosphonomethyl)phosphonic
 (medronic) acid comprising `handbell-like' [Pd{\m-CH~2~(PO~3~)~2~}]~3~
 units
;
_journal_coeditor_code           KU3068
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m242
_journal_page_last               m245
_journal_paper_doi               10.1107/S0108270112031368
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'K2 [Ni (H2 O)6]2 [Pd3 (C H2 O6 P2)3] , 6H2 O'
_chemical_formula_moiety         'C3 H33 K2 Ni2 O30 P6 Pd3, 6(H2 O)'
_chemical_formula_sum            'C3 H42 K2 Ni2 O36 P6 Pd3'
_chemical_formula_weight         1354.02
_chemical_name_systematic
;
dipotassium bis[hexaaquanickel(II)]
tris(\m~2~-methylenediphosphonato)tripalladium(II) hexahydrate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 128.934(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.6234(11)
_cell_length_b                   12.5467(6)
_cell_length_c                   16.0458(7)
_cell_measurement_reflns_used    8292
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      4.43
_cell_measurement_theta_min      2.22
_cell_volume                     3699.5(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction
;
SAINT-Plus (Bruker, 2007) and XPREP (Bruker, 2001)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF (Beurskens <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3231
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.97
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.028
_exptl_absorpt_correction_T_max  0.513808
_exptl_absorpt_correction_T_min  0.401868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Bruker, 2001)'
_exptl_crystal_colour            'translucent brown'
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.725
_refine_ls_extinction_coef       0.00016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         3231
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0215P)^2^+12.6038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0521
_reflns_number_gt                3019
_reflns_number_total             3231
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ku3068.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2018637
_cod_database_fobs_code          2018637