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_4506358
_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            'C217 H190 N46 Ni12 O25 S12'
_chemical_formula_weight         4931.23
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.759(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.243(3)
_cell_length_b                   22.585(2)
_cell_length_c                   35.586(3)
_cell_measurement_reflns_used    32637
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5010
_cell_measurement_theta_min      2.0787
_cell_volume                     23288(4)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            102899
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  0.6941
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             10124
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_platon_squeeze_details
;

SQUEEZE removed two disordered DMF and two disordered Py 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         1.299
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1264
_refine_ls_number_reflns         26377
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0530
_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^)+(0.1078P)^2^+42.0839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1696
_reflns_number_gt                23170
_reflns_number_total             26377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300483c_si_002.cif
_cod_data_source_block           complex_1
_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_sg_symbol_H-M      C2/c
_cod_database_code               4506358