Self-Assembly of Thiacalix[4]arene-Supported Nickel(II)/Cobalt(II) Complexes Sustained by in Situ Generated 5-Methyltetrazolate Ligand
Xiong, Kecai; Jiang, Feilong; Gai, Yanli; He, Zhangzhen; Yuan, Daqiang; Chen, Lian; Su, Kongzhao; Hong, Maochun; Crystal Growth & Design 12 (2012) 3335–; doi:10.1021/cg300483c

data_4506360
_publ_section_title
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 Self-Assembly of Thiacalix[4]arene-Supported Nickel(II)/Cobalt(II)
 Complexes Sustained by in Situ Generated 5-Methyltetrazolate Ligand
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_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3335
_journal_paper_doi               10.1021/cg300483c
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C160 H209 Co12 N35 O24 S12'
_chemical_formula_weight         4098.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   41.923(10)
_cell_length_b                   40.358(9)
_cell_length_c                   16.146(4)
_cell_measurement_reflns_used    50905
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4391
_cell_measurement_theta_min      2.5230
_cell_volume                     27318(11)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            152459
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.8164
_exptl_absorpt_correction_T_min  0.7562
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    0.9964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             8112
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;

SQUEEZE removed two disordered DMF molecules per formula unit. 
This valueis calculated based upon volume/count_electrons analysis 
and TG-MS analysis.
See ref: a) 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; 
b)Y. F. Bi, S. C. Du and W. P. Liao, Chem. Commun., 2011, 47, 4724.
;
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         25320
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0949
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1808P)^2^+14.1690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2817
_refine_ls_wR_factor_ref         0.3082
_reflns_number_gt                18642
_reflns_number_total             25320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300483c_si_002.cif
_cod_data_source_block           complex_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_original_cell_volume        27317(11)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4506360