Multimetallic Assemblies Using Piperazine-Based Dithiocarbamate Building Blocks
James D. E. T. Wilton-Ely; Dina Solanki; Edward R. Knight; Katherine B. Holt; Amber L. Thompson; Graeme Hogarth; Inorganic Chemistry 47 (2008) 9642–9653; doi:10.1021/ic800398b

data_4305401
_publ_contact_author_address
;
Chemistry Research Laboratory,
University of Oxford,
Mansfield Road, 
Oxford OX1 3TA. UK.
;
_publ_contact_author_email       james.wilton-ely@chem.ox.ac.uk
_publ_contact_author_name        'Dr. James D. Wilton-Ely'
_publ_section_title
;
Multimetallic Assemblies Using Piperazine-Based Dithiocarbamate Building
Blocks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9642
_journal_page_last               9653
_journal_paper_doi               10.1021/ic800398b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
'2(C32 H36 N2 Ni1 P1 S1), 1.5(B F4), C H Cl3, C H2 Cl2, Cl0.5'
_chemical_formula_sum            'C66 H75 B1.5 Cl5.5 F6 N4 Ni2 P4 S4'
_chemical_formula_weight         1619.03
_chemical_melting_point          ?
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.5845(13)
_cell_length_b                   24.5845(13)
_cell_length_c                   12.6638(10)
_cell_measurement_reflns_used    6900
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.652
_cell_measurement_theta_min      2.343
_cell_volume                     7654.0(8)
_computing_cell_refinement       'SMART-NT (Bruker, 2000)'
_computing_data_collection       'SMART-NT (Bruker, 2000)'
_computing_data_reduction        'SAINT-NT (Bruker, 2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       \w-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  0.0840
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25910
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G.M.Sheldrick, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         7840
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.2026
_reflns_number_gt                5542
_reflns_number_total             7840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800398b_si_003.cif
_cod_data_source_block           16a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C66 H75 B1.50 Cl5.50 F6 N4 Ni2 P4 S4'
_cod_database_code               4305401