Synthesis and Structure of Organic-Soluble Binuclear Molecular Phosphonates of Tantalum, Molybdenum, and Tungsten
Olexandr I. Guzyr; Rolf Siefken; Debashis Chakraborty; Herbert W. Roesky; Markus Teichert; Inorganic Chemistry 39 (2000) 1680–1683; doi:10.1021/ic990966f

data_4320866
_publ_contact_author
;
      Herbert W. Roesky
      Institut f\"ur Anorganische Chemie
      Universit\"at G\"ottingen
      Tammannstr. 4
      37077 G\"ottingen
      Germany
;
_publ_contact_author_email       agouzyr@gwdg.de
_publ_contact_author_fax         '049 551 393373'
_publ_contact_author_phone       '049 551 393001'
_publ_section_title
;
 Synthesis and Structure of Organic-Soluble Binuclear Molecular
 Phosphonates of Tantalum, Molybdenum, and Tungsten
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1680
_journal_page_last               1683
_journal_paper_doi               10.1021/ic990966f
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C40 H76 O15 P4 Ta2'
_chemical_formula_weight         1282.79
_chemical_name_systematic
;
 compound 2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.875(3)
_cell_length_b                   42.072(9)
_cell_length_c                   10.394(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      1.78
_cell_volume                     4989(2)
_computing_cell_refinement       'Bruker SAINT (V. 5.00, Bruker 1998)'
_computing_data_collection       'Siemens SMART (V. 4.202, Siemens 1996)'
_computing_data_reduction        'Bruker SAINT (V. 5.00, Bruker 1998)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 5.10)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type
'Stoe-Siemens-Huber four circle diffractometer'
_diffrn_measurement_method       'phi scan'
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            68445
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    4.572
_exptl_absorpt_correction_T_max  0.7402
_exptl_absorpt_correction_T_min  0.2975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.336
_refine_diff_density_min         -2.060
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.476
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.459
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+47.7568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                8164
_reflns_number_total             8756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990966f_1.cif
_cod_data_source_block           etoile
_cod_original_cell_volume        4989.5(19)
_cod_database_code               4320866