New Structural Forms in Molecular Metal Phosphonates: Novel Tri- and Hexanuclear Zinc(II) Cages Containing Phosphonate and Pyrazole Ligands
Vadapalli Chandrasekhar; Savariraj Kingsley; Brian Rhatigan; Matthew K. Lam.; Arnold L. Rheingold; Inorganic Chemistry 41 (2002) 1030–1032; doi:10.1021/ic011154y

data_4317668
_publ_contact_author
; 
     Chandrasekhar. V
     Department of Chemistry
     IIT, Kanpur 208 016
     India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91 512 597 436'
_publ_contact_author_phone       '+91 512 597 435'
_publ_section_title
;
 New Structural Forms in Molecular Metal Phosphonates: Novel Tri- and
 Hexanuclear Zinc(II) Cages Containing Phosphonate and Pyrazole Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1030
_journal_page_last               1032
_journal_paper_doi               10.1021/ic011154y
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C64 H84 Cl4 N16 O12 P4 Zn6, 4(C6 H6)'
_chemical_formula_sum            'C88 H108 Cl4 N16 O12 P4 Zn6'
_chemical_formula_weight         2239.90
_chemical_melting_point          168
_chemical_name_common            6Zn-cluster
_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                97.4881(50)
_cell_angle_beta                 94.3542(70)
_cell_angle_gamma                112.0637(60)
_cell_formula_units_Z            1
_cell_length_a                   12.7594(20)
_cell_length_b                   14.5816(20)
_cell_length_c                   15.1866(20)
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      1.5
_cell_volume                     2572.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13321
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  0.8559
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.766
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         7392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.766
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0912
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+5.3350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3339
_refine_ls_wR_factor_ref         0.3484
_reflns_number_gt                6986
_reflns_number_total             7392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011154y_1.cif
_cod_data_source_block           6ZN-CLUSTER
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_adp_type' tag value 'Uisi' was replaced with 'Uiso'
value.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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_original_cell_volume        2572.17(2)
_cod_database_code               4317668