Coordination modes of 2-mercaptonicotinic acid: synthesis and crystal structures of palladium(II), platinum(II), rhenium(III) and molybdenum(VI) complexes
Susana M. O. Quintal; Helena I. S. Nogueira; Vitor Félix; Michael G. B. Drew; J. Chem. Soc., Dalton Trans.  (2002) 4479–4487; doi:10.1039/b206101e

data_7011945
_publ_section_title
;
 Coordination modes of 2-mercaptonicotinic acid: synthesis and crystal
 structures of palladium(II), platinum(II), rhenium(III) and
 molybdenum(VI) complexes
;
_journal_issue                   23
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4479
_journal_page_last               4487
_journal_paper_doi               10.1039/b206101e
_journal_year                    2002
_chemical_formula_sum            'C45 H42.5 I2 N2 O3.5 P2 Re S'
_chemical_formula_weight         1201.31
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.26(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.068(16)
_cell_length_b                   23.579(26)
_cell_length_c                   18.371(24)
_cell_measurement_temperature    293(2)
_cell_volume                     4766(11)
_computing_molecular_graphics    'Platon (Spek, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'Mar research image plate system'
_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    0.0433
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8431
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    3.998
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2326
_refine_diff_density_max         2.094
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         8431
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0004P)^2^+148.8310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                6691
_reflns_number_total             8431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206101e.txt
_cod_data_source_block           compound_7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0004P)^2^+148.8310P] 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^)+(0.0004P)^2^+148.8310P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4764(11)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C45 H42.50 I2 N2 O3.50 P2 Re S'
_cod_database_code               7011945