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_4323122
_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_sum            'C24 H38 N2 Ni2 O4 S4'
_chemical_formula_weight         664.22
_chemical_name_systematic
;
 ?
;
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0841(3)
_cell_length_b                   14.4948(4)
_cell_length_c                   16.7751(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.41
_cell_measurement_theta_min      2.19
_cell_volume                     2938.27(13)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      133(2)
_diffrn_measurement_device       'Siemens SAMRT-CCD'
_diffrn_measurement_method       '\w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3863
_diffrn_reflns_theta_max         29.41
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.598
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       parallelepied
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00045(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.129
_refine_ls_goodness_of_fit_obs   1.163
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_restrained_S_obs      1.163
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_obs          0.0370
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+3.2769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0697
_refine_ls_wR_factor_obs         0.0653
_reflns_number_observed          3269
_reflns_number_total             3863
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9802956_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+3.2769P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+3.2769P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323122