Unique formation of two high-nuclearity metallamacrocycles from a mononuclear complex [Zn(dmpzdtc)2] (dmpzdtc=3,5-dimethylpyrazole-1-dithiocarboxylate) via CS2 elimination.
Li, Hong-Xi; Wu, Hua-Zhou; Zhang, Wen-Hua; Ren, Zhi-Gang; Zhang, Yong; Lang, Jian-Ping; Chemical communications (Cambridge, England)  (2007) 5052–5054; doi:10.1039/b710787k

data_7102327
_publ_section_title
;
 Unique formation of two high-nuclearity metallamacrocycles from a
 mononuclear complex [Zn(dmpzdtc)2]
 (dmpzdtc=3,5-dimethylpyrazole-1-dithiocarboxylate) via CS2
 elimination.
;
_journal_issue                   47
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5052
_journal_page_last               5054
_journal_paper_doi               10.1039/b710787k
_journal_year                    2007
_chemical_formula_moiety         'C60 H88 N24 O4 Zn8, 2(C2 H4 Br2)'
_chemical_formula_sum            'C64 H96 Br4 N24 O4 Zn8'
_chemical_formula_weight         2108.37
_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                64.53(3)
_cell_angle_beta                 81.38(3)
_cell_angle_gamma                68.43(3)
_cell_formula_units_Z            1
_cell_length_a                   10.577(2)
_cell_length_b                   14.267(3)
_cell_length_c                   16.194(3)
_cell_measurement_reflns_used    6223
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.0088
_cell_volume                     2051.6(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_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  0.0697
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20246
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.303
_exptl_absorpt_correction_T_max  0.6529
_exptl_absorpt_correction_T_min  0.4489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.353
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7469
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+7.0190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.2042
_reflns_number_gt                5297
_reflns_number_total             7469
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b710787k.txt
_cod_data_source_block           2
_cod_database_code               7102327