Synthesis and structural and magnetic characterisation of cobalt(ii)‒sodium phosphonate cage compounds
Langley, Stuart; Helliwell, Madeleine; Sessoli, Roberta; Teat, Simon J.; Winpenny, Richard E. P.; Dalton Transactions  (2009) 3102–3110; doi:10.1039/b819976k

data_7001034
_publ_section_title
;
 Synthesis and structural and magnetic characterisation of
 cobalt(ii)--sodium phosphonate cage compounds
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              3102
_journal_page_last               3110
_journal_paper_doi               10.1039/b819976k
_journal_year                    2009
_chemical_formula_sum            'C153 H129.5 Cl24 Co15 N37.5 Na O39.5 P3'
_chemical_formula_weight         4976.09
_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                 117.574(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   49.035(3)
_cell_length_b                   25.398(2)
_cell_length_c                   40.235(3)
_cell_measurement_reflns_used    7208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.54
_cell_measurement_theta_min      2.08
_cell_volume                     44417(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2111
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31826
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             19960
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2346
_refine_ls_number_reflns         31826
_refine_ls_number_restraints     1428
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1990
_refine_ls_wR_factor_ref         0.2123
_reflns_number_gt                15308
_reflns_number_total             31826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b819976k.txt
_cod_data_source_block           repw69sq
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C153 H129.50 Cl24 Co15 N37.50 Na O39.50 P3'
_cod_database_code               7001034