Solid state coordination chemistry of metal-azolate compounds: Structural consequences of incorporation of phosphate components in the Co(II)/4-pyridyltetrazolate/phosphate system
Kari Darling; Jon Zubieta; Inorganica Chimica Acta 394 (2013) 512–518; doi:10.1016/j.ica.2012.08.030

data_1512781
_publ_section_title
;
 Solid state coordination chemistry of metal-azolate compounds: Structural
 consequences of incorporation of phosphate components in the
 Co(II)/4-pyridyltetrazolate/phosphate system
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              512
_journal_page_last               518
_journal_paper_doi               10.1016/j.ica.2012.08.030
_journal_volume                  394
_journal_year                    2013
_chemical_formula_moiety         'C12 H18 Co3 N10 O12 P2'
_chemical_formula_sum            'C12 H18 Co3 N10 O12 P2'
_chemical_formula_weight         733.09
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9683(8)
_cell_length_b                   14.1302(16)
_cell_length_c                   22.426(3)
_cell_measurement_reflns_used    1002
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.97
_cell_volume                     2208.1(5)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1998)'
_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2006)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19788
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    2.461
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1998)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          .12
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2689
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+2.5686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                2332
_reflns_number_total             2689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-512-518-2.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1512781