Zinc Diphosphonates Templated by Organic Amines: Syntheses and Characterizations of [NH3(CH2)2NH3]Zn(hedpH2)2.2H2O and [NH3(CH2)nNH3]Zn2(hedpH)2.2H2O (n= 4, 5, 6) (hedp = 1-Hydroxyethylidenediphosphonate)
Hui-Hua Song; Li-Min Zheng; Zheming Wang; Chun-Hua Yan; Xin; Inorganic Chemistry 40 (2001) 5024–5029; doi:10.1021/ic010033v

data_4320239
_publ_section_title
;
 Zinc Diphosphonates Templated by Organic Amines: Syntheses and
 Characterizations of [NH3(CH2)2NH3]Zn(hedpH2)2.2H2O and
 [NH3(CH2)nNH3]Zn2(hedpH)2.2H2O (n= 4, 5, 6) (hedp =
 1-Hydroxyethylidenediphosphonate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5024
_journal_page_last               5029
_journal_paper_doi               10.1021/ic010033v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C9 H30 N2 O16 P4 Zn2'
_chemical_formula_weight         676.97
_chemical_name_systematic
;
  ?
;
_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                 99.1821(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.5251(2)
_cell_length_b                   12.5968(3)
_cell_length_c                   16.1705(5)
_cell_measurement_reflns_used    20022
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.02
_cell_measurement_theta_min      3.48
_cell_volume                     1111.02(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 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      293(2)
_diffrn_detector_area_resol_mean 0.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20022
_diffrn_reflns_theta_full        32.02
_diffrn_reflns_theta_max         32.02
_diffrn_reflns_theta_min         3.48
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.528
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0142(12)
_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   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3850
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.9797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                2976
_reflns_number_total             3850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010033v_3.cif
_cod_data_source_block           '[NH3(CH2)5NH3]Zn2(hedpH)2.2H2O_(znpen)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320239