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_7001032
_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            'C156 H134 Cl30 Co14 N22 Na4 O48 P6'
_chemical_formula_weight         5251.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.740(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.3288(9)
_cell_length_b                   26.0845(11)
_cell_length_c                   22.1377(10)
_cell_measurement_reflns_used    5283
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.84
_cell_measurement_theta_min      2.36
_cell_volume                     10571.9(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART Proteun 200 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6934
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_sigmaI/netI    0.1209
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38913
_diffrn_reflns_theta_full        24.09
_diffrn_reflns_theta_max         24.09
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.575
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5260
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1303
_refine_ls_number_reflns         17235
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.101
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1666
_reflns_number_gt                11997
_reflns_number_total             17235
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b819976k.txt
_cod_data_source_block           sl18
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7001032