Reactivity of 2-Pyridinecarboxylic Esters with Cadmium(II) Halides: Study of 113Cd NMR Solid State Spectra and Crystal Structures of Hexacoordinated Complexes [CdI2(C5H4NCOOMe)2] and [CdI2(C5H4NCOOPrn)2]
Ricard March; Josefina Pons; Josep Ros; William Clegg; Angel Álvarez-Larena; Joan Francesc Piniella; Jesus Sanz; Inorganic Chemistry 42 (2003) 7403–7409; doi:10.1021/ic0206387

data_4312458
_publ_section_title
;
 Reactivity of 2-Pyridinecarboxylic Esters with Cadmium(II) Halides: Study
 of 113Cd NMR Solid State Spectra and Crystal Structures of
 Hexacoordinated Complexes [CdI2(C5H4NCOOMe)2] and [CdI2(C5H4NCOOPrn)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7403
_journal_page_last               7409
_journal_paper_doi               10.1021/ic0206387
_journal_volume                  42
_journal_year                    2003
_chemical_formula_structural
'[Cd ((C5 H4 N) (C2 H3 O2))2  I2] (C H4 O)0.3'
_chemical_formula_sum            'C14.3 H15.2 Cd I2 N2 O4.3'
_chemical_formula_weight         650.08
_chemical_name_systematic
;
Diiodo-[bis[methyl-2-pyridinecarboxylate\k^2^N,O]cadmium(II)
0.3 methanol solvate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.91(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.124(1)
_cell_length_b                   15.546(1)
_cell_length_c                   12.385(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     1949.0(3)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega/2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3422
_diffrn_reflns_theta_full        24.93
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.308
_exptl_absorpt_correction_T_max  0.547
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.215
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1214
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3422
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+1.1503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                2519
_reflns_number_total             3422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0206387_1.cif
_cod_data_source_block           compound10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+1.1503P] 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^)+(0.0405P)^2^+1.1503P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C14.30 H15.20 Cd I2 N2 O4.30'
_cod_database_code               4312458