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_4320240
_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            'C10 H32 N2 O16 P4 Zn2'
_chemical_formula_weight         691.00
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                81.9822(19)
_cell_angle_beta                 89.4348(17)
_cell_angle_gamma                79.679(2)
_cell_formula_units_Z            2
_cell_length_a                   5.4785(2)
_cell_length_b                   14.1940(5)
_cell_length_c                   16.0682(6)
_cell_measurement_reflns_used    23456
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      3.62
_cell_volume                     1217.11(8)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Denzo & maXus'
_computing_molecular_graphics    'Bruker SHELXTL (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 0.76
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23456
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.62
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.309
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing (1995, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0053(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   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5676
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0435P)^2^+1.2462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                4447
_reflns_number_total             5676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010033v_4.cif
_cod_data_source_block           '[NH3(CH2)6NH3]Zn2(hedpH)2.2H2O_(znhn)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
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_cod_database_code               4320240