The synthesis and structure of a neutral tetranuclear zinc(II) complex [Zn4(L)4] [LH2 = N,N-bis(2-mercaptoethyl)benzylamine]
Spencer, Douglas J. E.; Blake, Alexander J.; Parsons, Simon; Schröder, Martin; Journal of the Chemical Society, Dalton Transactions  (1999) 1041–; doi:10.1039/a901251f

data_7027312
_publ_section_title
;
 The synthesis and structure of a neutral tetranuclear zinc(II) complex
 [Zn4(L)4] [LH2&#x2005;=&#x2005;N,N-bis(2-mercaptoethyl)benzylamine]
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1041
_journal_paper_doi               10.1039/a901251f
_journal_year                    1999
_chemical_formula_moiety         'C44 H60 N4 S8 Zn4, 0.5 C4 H10 O'
_chemical_formula_sum            'C46 H65 N4 O0.5 S8 Zn4'
_chemical_formula_weight         1199.98
_chemical_name_common            'Tetrazinc N-bis(mercaptoethyl)benzylamine'
_chemical_name_systematic
; 
 ? 
;
_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   'constrained to idealised positions'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier syntheses'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.90(2)
_cell_angle_beta                 88.70(2)
_cell_angle_gamma                62.674(14)
_cell_formula_units_Z            2
_cell_length_a                   13.926(3)
_cell_length_b                   14.593(3)
_cell_length_c                   14.631(5)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     2640.7(12)
_computing_cell_refinement       STADI-4
_computing_data_collection       'STADI-4 (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'SHELXTL/PC v5.03 (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9255
_diffrn_reflns_theta_full        70.21
_diffrn_reflns_theta_max         70.21
_diffrn_reflns_theta_min         4.54
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.297
_exptl_absorpt_correction_T_max  0.5690
_exptl_absorpt_correction_T_min  0.0922
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.86
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.45
_refine_diff_density_rms         0.09
_refine_ls_extinction_coef       0.00046(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9255
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.048P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                6150
_reflns_number_total             9255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            901251fsup1.cif
_cod_data_source_block           ZNNSPH
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (16
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.2 from 2011-04-26 (46
times).

'_geom_torsion_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.2 from 2011-04-26 (53 times).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.048P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.048P)^2^] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C46 H65 N4 O0.50 S8 Zn4'
_cod_database_code               7027312