Solvent-induced structural diversities from discrete cup-shaped Co8 clusters to Co8 cluster-based chains accompanied by in situ ligand conversion
Han, Song-De; Chen, Yong-Qiang; Zhao, Jiong-Peng; Liu, Sui-Jun; Miao, Xiao-Hong; Hu, Tong-Liang; Bu, Xian-He; CrystEngComm 16 (2014) 753–; doi:10.1039/c3ce42007h

data_7213907
_publ_section_title
;
 Solvent-induced structural diversities from discrete cup-shaped Co8
 clusters to Co8 cluster-based chains accompanied by in situ ligand
 conversion
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              753
_journal_paper_doi               10.1039/c3ce42007h
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C75 H56.5 Cl6 Co8 N31.5 O9'
_chemical_formula_sum            'C75 H56.5 Cl6 Co8 N31.5 O9'
_chemical_formula_weight         2227.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.252(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.867(4)
_cell_length_b                   17.119(3)
_cell_length_c                   28.504(5)
_cell_measurement_temperature    113(2)
_cell_volume                     8521(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  Multilayer
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            79926
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.17
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.782
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
; 

The PLATON SQUEEZE procedure was used to treat 
regions of diffuse solvent which could not be modeled 
properly in terms of atomic sites. Their contribution to 
the diffraction pattern was removed and modified F^2^ was
written to a new HKL file. The number of located electrons, 
748 in two voids per unit cell, is included in the formula, formula weight, 
calculated density, and F(000). The main framework of 1 is dianionic. 
Considering the sources of cation and the acidic reaction environment 
in the formation of 1, the negative charge may be balanced by two 
protonated water molecules. Similar cases are common in literature.
In the refinement of 1, highly disordered HBTA ligands are generated. 
However, these units cannot be modeled properly. There are four formula units 
in one unit cell. On base of charge balance considerations, volume/count_electrons 
analysis, TG analyses and elemental analyses, this residual electron density 
was assigned to two and half molecules of 1H-Benzotriazole (HBTA), 
two molecules of protonated water and one water molecule. 
So SQUEEZE removed these disordered units per unit cell. 
The tentative formula for compound 1 is presented as in the text.
See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake,
L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun.
2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare. Chem. Commun. 2008, 5987;
(c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang,
and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650; (d) C. Duan, M. Wei, D. Guo, 
C. He, and Q. Meng, J. Am. Chem. Soc. 2010, 132, 3321; 
(e) M. Wei, C. He, W. Hua, C. Duan, S. Li, and Q. Meng, J. Am. Chem. Soc. 2006, 128, 13318; 
(f) H. Zhang, Y. Lu, Z. Zhang, H. Fu, Y. Li, D. Volkmer, 
D. Denysenko and E.Wang, Chem. Commun. 2012, 48, 7295.
;
_refine_diff_density_max         1.601
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         20307
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+44.3964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2079
_reflns_number_gt                15545
_reflns_number_total             20307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42007h.txt
_cod_data_source_block           added_by_encifer
_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/RSC/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      'P 21/c'
_cod_database_code               7213907