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_4323074
_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)2, C8 Cu1 S4 N4 '
_chemical_formula_sum            'C36 H40 Cu Fe2 N6 S4'
_chemical_formula_weight         860.3
_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                 109.81(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.804(1)
_cell_length_b                   10.036(1)
_cell_length_c                   15.971(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    160
_cell_measurement_theta_max      48.0
_cell_measurement_theta_min      4.1
_cell_volume                     1930.8(4)
_diffrn_ambient_temperature      160
_diffrn_measurement_device       '  STOE IPDS '
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15403
_diffrn_reflns_theta_max         24.08
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.53
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            ' red-brown '
_exptl_crystal_density_diffrn    1.48
_exptl_crystal_description       ' platelet '
_exptl_crystal_F_000             888.64
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.80
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.0486
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         2792
_refine_ls_R_factor_obs          0.0364
_refine_ls_shift/esd_max         0.142227
_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         0.0328
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_observed          2792
_reflns_number_total             2931
_reflns_observed_criterion       >0.00\s(I)
_cod_data_source_file            ic9804317_1.cif
_cod_data_source_block           C36H40Cu1S4N6Fe2
_cod_original_cell_volume        1930.84
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C36 H40 Cu1 S4 N6 Fe2 '
_cod_database_code               4323074