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_4072639
_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 H51 Co4 O34 P8), 0.5(H2 O), 0.5(H2O)'
_chemical_formula_sum            'C39 H53 Co4 O35 P8'
_chemical_formula_weight         1565.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.855(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.6791(18)
_cell_length_b                   22.1307(18)
_cell_length_c                   29.632(2)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    103(1)
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.41
_cell_volume                     18017(2)
_computing_cell_refinement       'Bruker SMART v5.631 (Bruker, 2001b)'
_computing_data_collection       'Bruker SMART v5.631 (Bruker, 2001b)'
_computing_data_reduction
;
Bruker SAINT v6.45 (Bruker, 2002), Bruker XPREP v6.14 (Bruker, 2001a)
;
_computing_molecular_graphics    'Bruker SHELXTL v6.14 (Bruker, 2000a)'
_computing_publication_material  'Bruker SHELXTL v6.14 (Bruker, 2000a)'
_computing_structure_refinement  'Bruker SHELXTL v6.14 (Bruker, 2000a)'
_computing_structure_solution    'Bruker SHELXTL v6.14 (Bruker, 2000a)'
_diffrn_ambient_temperature      103(1)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            66066
_diffrn_reflns_theta_full        26.86
_diffrn_reflns_theta_max         26.86
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  variable
_diffrn_standards_number         2135
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10 (Bruker, 2000b)'
_exptl_crystal_colour            pale_orange
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             6368
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details
; 
see _refine_special_details
;
_refine_diff_density_max         0.798
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         18961
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0736P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                12707
_reflns_number_total             18961
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om060898msi20060930_121513.cif
_cod_data_source_block           ts007
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4072639