A trinuclear cobalt(III) phosphate complex with a novel molecular structure: Synthesis and crystal structure of {[Co(en)~2~]~3~(PO~4~)(HPO~4~)}~2~(H~2~PO~4~)Cl~7~.6H~2~O
Rajni Sharma; Raj Pal Sharma; Ritu Bala; Miguel Quirós; Juan M. Salas; Inorganic Chemistry Communications 9 (2006) 782–784; doi:10.1016/j.inoche.2006.04.001

data_1500008
_publ_contact_author_address
;
     Departamento de Qu\'imica Inorg\'anica
     Facultad de Ciencias
     Universidad de Granada
     18071 Granada
     SPAIN
;
_publ_contact_author_email       mquiros@ugr.es
_publ_contact_author_fax         34-58-248526
_publ_contact_author_name        'Miguel Quir\'os'
_publ_contact_author_phone       34-58-240441
_publ_section_title
;
 A trinuclear cobalt(III) phosphate complex with a novel molecular structure:
 Synthesis and crystal structure of
 {[Co(en)~2~]~3~(PO~4~)(HPO~4~)}~2~(H~2~PO~4~)Cl~7~.6H~2~O
;
_journal_name_full               'Inorganic Chemistry Communications'
_journal_page_first              782
_journal_page_last               784
_journal_paper_doi               10.1016/j.inoche.2006.04.001
_journal_volume                  9
_journal_year                    2006
_chemical_absolute_configuration unk
_chemical_formula_moiety
'2 (C12 H49 Co3 N12 O8 P2 4+), H2 O4 P -1, 7 (Cl 1-), 6 (H2 O)'
_chemical_formula_sum            'C24 H112 Cl7 Co6 N24 O26 P5'
_chemical_formula_weight         1909.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.230(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8349(9)
_cell_length_b                   18.7451(13)
_cell_length_c                   16.0020(11)
_cell_measurement_reflns_used    5189
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.6
_cell_volume                     3635.1(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22257
_diffrn_reflns_theta_full        26.90
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        -0.1
_diffrn_standards_number         687
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 The structure has been refined as a twin of the two enantiomers
 in identical proportions
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         14874
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0500P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                13711
_reflns_number_total             14874
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cohpo.cif
_cod_data_source_block           cohpo
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1500008