The role of deprotonation of the ligand on the structures of metal phosphonates: synthesis, characterization and crystal structures of two new metal diphosphonates with a 1D double chain and a 2D layer structure
Mao, Jiang-Gao; Wang, Zhike; Clearfield, Abraham; Journal of the Chemical Society, Dalton Transactions  (2002) 4457–; doi:10.1039/b204270n

data_7011808
_publ_section_title
;
 The role of deprotonation of the ligand on the structures of metal
 phosphonates: synthesis, characterization and crystal structures of
 two new metal diphosphonates with a 1D double chain and a 2D layer
 structure
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4457
_journal_paper_doi               10.1039/b204270n
_journal_year                    2002
_chemical_formula_sum            'C6 H24 Cd N2 O14 P4'
_chemical_formula_weight         584.55
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                82.408(7)
_cell_angle_beta                 73.694(7)
_cell_angle_gamma                89.773(7)
_cell_formula_units_Z            2
_cell_length_a                   9.418(4)
_cell_length_b                   9.948(4)
_cell_length_c                   10.574(5)
_cell_measurement_temperature    110(2)
_cell_volume                     941.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       'narrow frame method, hemisphere'
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6003
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0732P)^2^+4.6301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                3909
_reflns_number_total             4267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204270n.txt
_cod_data_source_block           mao12
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011808