Isolated Co15 Clusters and Their Assembly into a 3D Network: Conformation-Directed Synthesis
Zhi-Guo Gu; Slavi C. Sevov; Inorganic Chemistry 48 (2009) 8066–8068; doi:10.1021/ic9010778

data_4303081
_publ_section_title
;
Isolated Co15 Clusters and Their Assembly into a 3D Network:
Conformation-Directed Synthesis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8066
_journal_page_last               8068
_journal_paper_doi               10.1021/ic9010778
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C21 H101 Co7.5 N3 O66 P3'
_chemical_formula_weight         1986.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.037(2)
_cell_angle_beta                 107.798(2)
_cell_angle_gamma                101.151(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4481(8)
_cell_length_b                   15.5519(8)
_cell_length_c                   16.1103(8)
_cell_measurement_reflns_used    9528
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.39
_cell_volume                     3328.9(3)
_computing_cell_refinement       'Bruker SAINT v7.53A'
_computing_data_collection       'Bruker APEX-II v2008-6'
_computing_data_reduction        'Bruker SAINT v7.53A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of \w and \f-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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            99805
_diffrn_reflns_theta_full        27.23
_diffrn_reflns_theta_max         27.23
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    2.032
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5914
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2047
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         2.937
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         14551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1235P)^2^+4.2950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.1969
_reflns_number_gt                11357
_reflns_number_total             14551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9010778_si_002_1.cif
_cod_data_source_block           Co15cluster
_cod_original_formula_sum        'C21 H101 Co7.50 N3 O66 P3'
_cod_database_code               4303081