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_1512780
_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         'C18 H12 Co3 N15 O4 P'
_chemical_formula_sum            'C18 H12 Co3 N15 O4 P'
_chemical_formula_weight         710.19
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   22.202(2)
_cell_length_b                   22.202(2)
_cell_length_c                   4.3536(9)
_cell_measurement_reflns_used    990
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.97
_cell_volume                     1858.5(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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0908
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5807
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    2.111
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1998)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1059
_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .08
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1987
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                1744
_reflns_number_total             1987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-512-518-1.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        1858.4(5)
_cod_original_sg_symbol_H-M      R3
_cod_database_code               1512780