Molecular zinc phosphonates: synthesis and X-ray crystal structures of [[(ZnMe)4(THF)2][tBuPO3]2] and [[(ZnEt)3(Zn(THF))3][tBuPO3]4[mu3-OEt]].
Anantharaman, Ganapathi; Chandrasekhar, Vadapalli; Walawalkar, Mrinalini G.; Roesky, Herbert W.; Vidovic, Denis; Magull, Jorg; Noltemeyer, Mathias; Dalton transactions (Cambridge, England : 2003)  (2004) 1271–1275; doi:10.1039/b400168k

data_7014027
_publ_section_title
;
 Molecular zinc phosphonates: synthesis and X-ray crystal structures of
 [[(ZnMe)4(THF)2][tBuPO3]2] and
 [[(ZnEt)3(Zn(THF))3][tBuPO3]4[mu3-OEt]].
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1271
_journal_page_last               1275
_journal_paper_doi               10.1039/b400168k
_journal_year                    2004
_chemical_formula_sum            'C36 H80 O16 P4 Zn6'
_chemical_formula_weight         1285.10
_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                89.39(3)
_cell_angle_beta                 85.99(3)
_cell_angle_gamma                78.10(3)
_cell_formula_units_Z            2
_cell_length_a                   12.512(3)
_cell_length_b                   13.218(3)
_cell_length_c                   16.542(3)
_cell_measurement_temperature    133(2)
_cell_volume                     2670.4(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0981
_diffrn_reflns_av_sigmaI/netI    0.1142
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22491
_diffrn_reflns_theta_full        24.84
_diffrn_reflns_theta_max         24.84
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    2.830
_exptl_absorpt_correction_T_max  0.568
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   XPREP
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.783
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         9031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.783
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                5839
_reflns_number_total             9031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b400168k.txt
_cod_data_source_block           zincphosphonate3
_cod_original_cell_volume        2670.7(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7014027