Tracking the Formation of a Polynuclear Co16 Complex and Its Elimination and Substitution Reactions by Mass Spectroscopy and Crystallography
Yue-Qiao Hu; Ming-Hua Zeng; Kun Zhang; Sheng Hu; Fu-Fang Zhou; Mohamedally Kurmoo; Journal of the American Chemical Society 135 (2013) 7901–7908; doi:10.1021/ja3123784

data_4119798
_publ_contact_author_address
'No.15, Yucai Road, GuangXi Normal University, Guilin, China'
_publ_contact_author_email       ZMH@MAILBOX.GXNU.EDU.CN
_publ_contact_author_name        'Ming-Hua Zeng'
_publ_section_title
;
 Tracking the Formation of a Polynuclear Co16 Complex and Its Elimination
 and Substitution Reactions by Mass Spectroscopy and Crystallography
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7901
_journal_page_last               7908
_journal_paper_doi               10.1021/ja3123784
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C194 H144 Co16 N68 O47'
_chemical_formula_weight         5122.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.153(2)
_cell_length_b                   29.754(2)
_cell_length_c                   28.621(2)
_cell_measurement_temperature    150(2)
_cell_volume                     22272(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            60899
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.799
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_F_000             10368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1435
_refine_ls_number_reflns         21895
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1105P)^2^+78.9787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1793
_reflns_number_gt                18848
_reflns_number_total             21895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3123784_si_001.cif
_cod_data_source_block           Co16
_cod_original_cell_volume        22271(3)
_cod_database_code               4119798