High Nuclearity (Octa-, Dodeca-, and Pentadecanuclear) Metal (M = Co(II), Ni(II)) Phosphonate Cages: Synthesis, Structure, and Magnetic Behavior.
Sheikh, Javeed Ahmad; Adhikary, Amit; Jena, Himanshu Sekhar; Biswas, Soumava; Konar, Sanjit; Inorganic chemistry 53 (2014) 1606–1613; doi:10.1021/ic402673v

data_4337327
_publ_section_title
;
 High Nuclearity (Octa-, Dodeca-, and Pentadecanuclear) Metal (M = Co(II),
 Ni(II)) Phosphonate Cages: Synthesis, Structure, and Magnetic Behavior.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1606
_journal_page_last               1613
_journal_paper_doi               10.1021/ic402673v
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C94 H141 Ni8 O40 P2'
_chemical_formula_sum            'C94 H141 Ni8 O40 P2'
_chemical_formula_weight         2442.54
_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                 105.678(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   57.000(7)
_cell_length_b                   16.0479(18)
_cell_length_c                   30.275(3)
_cell_measurement_reflns_used    47156
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      2.23
_cell_volume                     26663(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.1074
_diffrn_reflns_av_sigmaI/netI    0.1360
_diffrn_reflns_limit_h_max       85
_diffrn_reflns_limit_h_min       -85
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            47156
_diffrn_reflns_theta_full        32.22
_diffrn_reflns_theta_max         32.22
_diffrn_reflns_theta_min         0.74
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cubic
_exptl_crystal_F_000             10232
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.769
_refine_diff_density_min         -2.100
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         43930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1895
_refine_ls_R_factor_gt           0.1228
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0040P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2646
_refine_ls_wR_factor_ref         0.2791
_reflns_number_gt                40309
_reflns_number_total             47156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402673v_si_004.cif
_cod_data_source_block           Complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4337327