Saccharinate as a Versatile Polyfunctional Ligand. Four Distinct Coordination Modes, Misdirected Valence, and a Dominant Aggregate Structure from a Single Reaction System
Larry R. Falvello; Julio Gomez; Isabel Pascual; Milagros Tomás; Esteban P. Urriolabeitia; Arthur J. Schultz; Inorganic Chemistry 40 (2001) 4455–4463; doi:10.1021/ic010300x

data_4320110
_publ_contact_author_address
; Department of Inorganic Chemistry
  University of Zaragoza
  Plaza San Francisco s/n
  E-50009 Zaragoza
  Spain
;
_publ_contact_author_fax         34()976761187
_publ_contact_author_name        'Larry R. Falvello'
_publ_contact_author_phone       34()976761179
_publ_section_title
;
 Saccharinate as a Versatile Polyfunctional Ligand. Four Distinct
 Coordination Modes, Misdirected Valence, and a Dominant Aggregate
 Structure from a Single Reaction System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4455
_journal_page_last               4463
_journal_paper_doi               10.1021/ic010300x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C14 H22 Cu N6 O7 S2'
_chemical_formula_weight         514.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                98.05(3)
_cell_angle_beta                 92.39(3)
_cell_angle_gamma                99.08(3)
_cell_formula_units_Z            2
_cell_length_a                   7.0450(10)
_cell_length_b                   10.578(2)
_cell_length_c                   13.967(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      15.1
_cell_measurement_theta_min      12.5
_cell_volume                     1015.5(3)
_computing_molecular_graphics    'SHELXTL Rel. 5.05/VMS (Siemens, 1996)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      566(2)
_diffrn_measurement_device       'Stoe AED-2'
_diffrn_measurement_method       'omega-2theta 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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3902
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       'regular block'
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.079
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         3418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_obs          0.0296
_refine_ls_shift/esd_max         -0.092
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.4258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0716
_refine_ls_wR_factor_obs         0.0668
_reflns_number_observed          3028
_reflns_number_total             3583
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010300x_5.cif
_cod_data_source_block           cpd7XRay
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Psi-scan'
changed to 'psi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.4258P] 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^)+(0.0314P)^2^+0.4258P] 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               4320110