Structural Studies of Bis-Catecholate, Bis-Dithiocatecholate, and Tetraalkoxy Diborane(4) Compounds
William Clegg; Mark R. J. Elsegood; Fiona J. Lawlor; Nicholas C. Norman; Nigel L. Pickett; Edward G. Robins; Andrew J. Scott; Paul Nguyen; Nicholas J. Taylor; Todd B. Marder; Inorganic Chemistry 37 (1998) 5289–5293; doi:10.1021/ic9804317

data_4323075
_publ_section_title
;
 Structural Studies of Bis-Catecholate, Bis-Dithiocatecholate, and
 Tetraalkoxy Diborane(4) Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5289
_journal_page_last               5293
_journal_paper_doi               10.1021/ic9804317
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source
;
metathesis reaction
;
_chemical_formula_moiety         ' C14 H20 Fe1 N1, C8 Ni1 S4 N4 '
_chemical_formula_sum            'C22 H20 Fe N5 Ni S4'
_chemical_formula_weight         597.3
_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
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 103.50(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.116(2)
_cell_length_b                   30.094(16)
_cell_length_c                   7.139(6)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    293
_cell_measurement_theta_max      10
_cell_measurement_theta_min      6
_cell_volume                     2531(3)
_diffrn_ambient_temperature      293
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.01
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7880
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        3.11
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.66
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '\y scan,(North et al, 1968)'
_exptl_crystal_colour            ' black '
_exptl_crystal_density_diffrn    1.55
_exptl_crystal_description       ' hexagonal bar '
_exptl_crystal_F_000             1204.13
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   0.9279
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         4295
_refine_ls_R_factor_obs          0.0461
_refine_ls_shift/esd_max         1.761349
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0331
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              42
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_observed          4295
_reflns_number_total             7338
_reflns_observed_criterion       >1.50\s(I)
_cod_data_source_file            ic9804317_2.cif
_cod_data_source_block           C22H20Ni1S4N5Fe1
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C22 H20 Ni1 S4 N5 Fe1 '
_cod_database_code               4323075