Synthesis and structure of the hexameric, dodecanuclear metallamacrocycle [(5-methyl-3-phenylpyrazole)2Zn2(OCH2CH2S)]6
Puerta, David T.; Cohen, Seth M.; Chemical Communications (Cambridge, United Kingdom)  (2003) 1278–1279; doi:10.1039/b300453h

data_7113790
_publ_section_title
;
 Synthesis and structure of the hexameric, dodecanuclear metallamacrocycle
 [(5-methyl-3-phenylpyrazole)2Zn2(OCH2CH2S)]6
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   11
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1278
_journal_page_last               1279
_journal_paper_doi               10.1039/b300453h
_journal_year                    2003
_chemical_formula_moiety         '[Zn6(5,3-mppz)6(b-me)]2'
_chemical_formula_sum            'C132 H132 N24 O6 S6 Zn12'
_chemical_formula_weight         3127.42
_chemical_name_systematic
;
[(5,3-methylphenylpyrazole)2Zn2(OCH2CH2S)]6
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   29.6563(18)
_cell_length_b                   29.6563(18)
_cell_length_c                   19.187(3)
_cell_measurement_temperature    100(2)
_cell_volume                     14614(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.706
_diffrn_measured_fraction_theta_max 0.706
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.1274
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24253
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.556
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             4788
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          25.056
_refine_ls_shift/su_mean         0.116
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0907P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                3177
_reflns_number_total             5294
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103663
_cod_data_source_file            b300453h.txt
_cod_data_source_block           finalring
_cod_original_cell_volume        14614(2)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7113790