Organometallic Supramolecular Mixed-Valence Cobalt(I)/Cobalt(II) Aquo Complexes Stabilized with the Water-Soluble Phosphine Ligandp-TPPTP (p-triphenylphosphine triphosphonic acid)
Schull, Terence L.; Henley, Leila; Deschamps, Jeffrey R.; Butcher, Ray J.; Maher, Dermot P.; Klug, Christopher A.; Swider-Lyons, Karen; Dressick, Walter J.; Bujoli, Bruno; Greenwood, Andrew E.; Congiardo, Laura K. Byington; Knight, D. Andrew; Organometallics 26 (2007) 2272–; doi:10.1021/om060898m

data_4072638
_publ_section_title
;
 Organometallic Supramolecular Mixed-Valence Cobalt(I)/Cobalt(II) Aquo
 Complexes Stabilized with the Water-Soluble Phosphine Ligandp-TPPTP
 (p-triphenylphosphine triphosphonic acid)
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2272
_journal_paper_doi               10.1021/om060898m
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C39 H24 Co O21 P8, 5(Co), 45.87(H2 O)'
_chemical_formula_sum            'C39 H115.74 Co6 O66.87 P8'
_chemical_formula_weight         2268.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.086(10)
_cell_angle_beta                 111.634(15)
_cell_angle_gamma                104.923(13)
_cell_formula_units_Z            2
_cell_length_a                   15.744(10)
_cell_length_b                   17.892(9)
_cell_length_c                   18.302(9)
_cell_measurement_reflns_used    8714
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.39
_cell_volume                     4469(4)
_computing_cell_refinement       'Bruker SMART v5.059 (Bruker, 1999)'
_computing_data_collection       'Bruker SMART v5.059 (Bruker, 1999)'
_computing_data_reduction
;
Bruker SAINT v6.02A (Bruker, 2000a), Bruker XPREP v5.1 (Bruker, 1997)
;
_computing_molecular_graphics    'Bruker Shelxtl v6.10 (Bruker, 2000b)'
_computing_publication_material  'Bruker Shelxtl v6.10 (Bruker, 2000b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.1205
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45884
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.22
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  variable
_diffrn_standards_number         1042
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.01 (Bruker, 2000c)'
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisim
_exptl_crystal_F_000             2333.4
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.424
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         21450
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          4.247
_refine_ls_shift/su_mean         0.064
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                13340
_reflns_number_total             21454
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om060898msi20060930_121345.cif
_cod_data_source_block           ts006b
_cod_original_formula_sum        'C39 H115.74  Co6 O66.87 P8'
_cod_database_code               4072638