Synthesis, Characterization, and Crystal Structures of Two New Divalent Metal Complexes of N,N'-Bis(phosphonomethyl)-1,10-diaza-18-crown-6: A Hydrogen-Bonded 1D Array and a 3D Network with a Large Channel
Jiang-Gao Mao; Zhike Wang; Abraham Clearfield; Inorganic Chemistry 41 (2002) 3713–3720; doi:10.1021/ic0200601

data_4318206
_publ_section_title
;
 Synthesis, Characterization, and Crystal Structures of Two New Divalent
 Metal Complexes of N,N'-Bis(phosphonomethyl)-1,10-diaza-18-crown-6: A
 Hydrogen-Bonded 1D Array and a 3D Network with a Large Channel
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3713
_journal_page_last               3720
_journal_paper_doi               10.1021/ic0200601
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C15 H60 Cd2.75 N3.5 O29.5 P2'
_chemical_formula_weight         1132.71
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.8150(9)
_cell_length_b                   20.8150(9)
_cell_length_c                   18.5846(12)
_cell_measurement_temperature    110(2)
_cell_volume                     8052.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       'narrow frame method'
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22384
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4580
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.572
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         8276
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1407P)^2^+31.1959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2293
_reflns_number_gt                6189
_reflns_number_total             8276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0200601_2.cif
_cod_data_source_block           maoc11
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C15 H60 Cd2.75 N3.50 O29.50 P2'
_cod_database_code               4318206