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_4320106
_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            'C61 H49 Cu N O3 P3 S'
_chemical_formula_weight         1032.52
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.294(3)
_cell_length_b                   19.784(2)
_cell_length_c                   24.974(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.8
_cell_measurement_theta_min      12.0
_cell_volume                     10027(2)
_computing_cell_refinement       'CAD4/PC V1.2 (Nonius, 1993)'
_computing_data_collection       'CAD4/PC V1.2 (Nonius, 1993)'
_computing_data_reduction        'XCAD4B (Harms, 1994)'
_computing_molecular_graphics    'SHELXTL Rel. 5.05/VMS (Siemens, 1996)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       'omega-theta 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    0.5960
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8801
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.01
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8801
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.4021
_refine_ls_R_factor_gt           0.1040
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1984
_reflns_number_gt                2527
_reflns_number_total             8801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010300x_1.cif
_cod_data_source_block           cpd3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.0000P] 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^)+(0.0222P)^2^+0.0000P] 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               4320106