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_4312459
_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) (C4 H7 O2))2  I2]'
_chemical_formula_sum            'C18 H22 Cd I2 N2 O4'
_chemical_formula_weight         696.58
_chemical_name_systematic
;
Diiodo-[bis[n-propyl-2-pyridinecarboxylate\k^2^N,O]cadmium(II)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.198(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8997(6)
_cell_length_b                   15.3101(10)
_cell_length_c                   17.8929(11)
_cell_measurement_reflns_used    11934
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.33
_cell_volume                     2383.0(3)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14439
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.530
_exptl_absorpt_correction_T_max  0.217
_exptl_absorpt_correction_T_min  0.125
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00076(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.176
_refine_ls_goodness_of_fit_obs   1.157
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_restrained_S_obs      1.157
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_obs          0.0231
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+3.0960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0553
_refine_ls_wR_factor_obs         0.0524
_reflns_number_observed          5088
_reflns_number_total             5426
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0206387_2.cif
_cod_data_source_block           compound12
_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^)+(0.0178P)^2^+3.0960P] 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^)+(0.0178P)^2^+3.0960P] 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               4312459