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_4337325
_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         'C108 H156 Ni12 O58 P4, 3(C2 H3 N), 6.5(O)'
_chemical_formula_sum            'C114 H165 N3 Ni12 O64.5 P4'
_chemical_formula_weight         3437.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   19.7023(5)
_cell_length_b                   19.7023(5)
_cell_length_c                   52.319(2)
_cell_measurement_reflns_used    2635
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      22.01
_cell_measurement_theta_min      2.01
_cell_volume                     17588.3(9)
_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, 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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            82767
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cubic
_exptl_crystal_F_000             7128
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         12529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+242.1672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2117
_reflns_number_gt                10688
_reflns_number_total             12529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402673v_si_003.cif
_cod_data_source_block           j-complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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 

2021-04-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C228 H330 N6 Ni24 O129 P8'
_cod_original_formula_weight         6875.29
_cod_original_formula_moiety     '2(C108 H156 Ni12 O58 P4), 6(C2 H3 N), 13(O)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        17588.5(13)
_cod_original_sg_symbol_H-M      'P -3 c1'
_cod_database_code               4337325