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_7014026
_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            'C20 H46 O8 P2 Zn4'
_chemical_formula_weight         737.99
_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                 95.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.933(2)
_cell_length_b                   11.311(2)
_cell_length_c                   13.865(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     1550.4(5)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE AED2'
_diffrn_measurement_method       'profile fit'
_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  0.1860
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3640
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.197
_exptl_absorpt_correction_T_max  0.2500
_exptl_absorpt_correction_T_min  0.1423
_exptl_absorpt_correction_type   'azimuthal scans'
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             760
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.60
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+1.2743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                2369
_reflns_number_total             2728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b400168k.txt
_cod_data_source_block           zincphosphonate(2)
_cod_original_cell_volume        1550.3(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7014026