Coordination Chemistry of a Tripodal S2ON Ligand: Syntheses, Structures, and Reactivity of the Molybdenum(VI) and Nickel(II) Complexes of Bis(2-mercaptoethyl)-2-amino-4-methylphenol (H3btap) and Comparison to V^V^O(btap)
Charles R. Cornman; Kevin L. Jantzi; Joseph I. Wirgau; Thad C. Stauffer; Jeff W. Kampf; Paul D. Boyle; Inorganic Chemistry 37 (1998) 5851–5855; doi:10.1021/ic9802956

data_4323123
_publ_contact_author_address
;Department of Chemistry
Box 8204
North Carolina State University
Raleigh, NC 27695-8204
;
_publ_contact_author_email       cornman@chemdept.chem.ncsu.edu
_publ_contact_author_fax         1(919)5155079
_publ_contact_author_name        'Charles R. Cornman'
_publ_contact_author_phone       1(919)5153209
_publ_section_title
;
 Coordination Chemistry of a Tripodal S2ON Ligand: Syntheses, Structures,
 and Reactivity of the Molybdenum(VI) and Nickel(II) Complexes of
 Bis(2-mercaptoethyl)-2-amino-4-methylphenol (H3btap) and Comparison to
 V^V^O(btap)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5851
_journal_page_last               5855
_journal_paper_doi               10.1021/ic9802956
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'Mo K S2 O4 N C11 H16 '
_chemical_formula_sum            'C11 H16 K Mo N O4 S2'
_chemical_formula_weight         425.41
_chemical_name_common            K[Mo^VI^O2(btap)]
_chemical_name_systematic
;
Potassium bis(2-mercaptoethyl)-2-amino-4-methylphenoldioxomolybdate(VI)
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   6.6596(9)
_cell_length_b                   13.7446(9)
_cell_length_c                   32.992(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    148
_cell_measurement_theta_max      19.00
_cell_measurement_theta_min      14.00
_cell_volume                     3019.9(5)
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      148
_diffrn_measurement_device       'Nonius CAD-4    '
_diffrn_measurement_method       'Omega scan b/P/b        '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2630
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_time  80
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.40
_exptl_absorpt_correction_T_max  .9998
_exptl_absorpt_correction_T_min  .8795
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'NRCVAX ABSORP'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       needle
_exptl_crystal_F_000             1701.12
_exptl_crystal_size_max          .36
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .04
_refine_diff_density_max         .72
_refine_diff_density_min         -.67
_refine_ls_goodness_of_fit_obs   1.05
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         1985
_refine_ls_R_factor_all          .042
_refine_ls_R_factor_obs          .041
_refine_ls_shift/esd_max         .004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     '1/(\s^2^(F)+ .0010F^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .050
_refine_ls_wR_factor_obs         .049
_reflns_number_observed          1991
_reflns_number_total             2630
_reflns_observed_criterion       'Inet > 1.0\s(Inet)'
_cod_data_source_file            ic9802956_2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'Mo K S2 O4 N C11 H16 '
_cod_database_code               4323123