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_4323076
_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 Pt1 S4 N4 '
_chemical_formula_sum            'C22 H20 Fe N5 Pt S4'
_chemical_formula_weight         733.61
_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                 103.97(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   12.119(4)
_cell_length_b                   30.112(4)
_cell_length_c                   7.244(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      11
_cell_measurement_theta_min      6
_cell_volume                     2565.3(17)
_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  0.02
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4730
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        1.88
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.49
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '\y scan,(North et al, 1968)'
_exptl_crystal_colour            ' black '
_exptl_crystal_density_diffrn    1.90
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             1413.95
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.14
_refine_diff_density_min         -1.00
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.0594
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         2687
_refine_ls_R_factor_obs          0.0508
_refine_ls_shift/esd_max         0.432918
_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         0.0422
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_observed          2687
_reflns_number_total             4511
_reflns_observed_criterion       >1.50\s(I)
_cod_data_source_file            ic9804317_3.cif
_cod_data_source_block           C22H20Pt1S4N5Fe1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2565(2)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C22 H20 Pt1 S4 N5 Fe1 '
_cod_database_code               4323076