Hydrido Copper Clusters Supported by Dithiocarbamates: Oxidative Hydride Removal and Neutron Diffraction Analysis of [Cu7(H){S2C(aza-15-crown-5)}6]
Ping-Kuei Liao; Ching-Shiang Fang; Alison J. Edwards; Samia Kahlal; Jean-Yves Saillard; C. W. Liu; Inorganic Chemistry 51 (2012) 6577–6591; doi:10.1021/ic300135w

data_4329446
_publ_contact_author_address
; 
 Bragg Institute 
 Australian Nuclear Science and Technology Organization
 Locked Bag 2001 
 Kirrawee, N.S.W. 22342
 Australia 
;
_publ_contact_author_email       alison.edwards@ansto.gov.au
_publ_contact_author_fax         '+61 2 97173607'
_publ_contact_author_name        'Alison Edwards'
_publ_contact_author_phone       '+61 2 97177247'
_publ_section_title
;
 Hydrido Copper Clusters Supported by Dithiocarbamates: Oxidative Hydride
 Removal and Neutron Diffraction Analysis of
 [Cu7(H){S2C(aza-15-crown-5)}6]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6577
_journal_page_last               6591
_journal_paper_doi               10.1021/ic300135w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C43 H86 Cl3 Cu8 F6 N6 P S12'
_chemical_formula_weight         1831.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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            4
_cell_length_a                   15.2054(4)
_cell_length_b                   15.2054(4)
_cell_length_c                   37.4914(9)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.25
_cell_volume                     7506.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            43877
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.730
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.860
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0987P)^2^+15.2207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1664
_reflns_number_gt                4243
_reflns_number_total             4941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300135w_si_002_1.cif
_cod_data_source_block           1H
_cod_database_code               4329446