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_4329448
_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            'C69 H127 Cu7 N6 O25 S12'
_chemical_formula_weight         2270.27
_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                92.371(2)
_cell_angle_beta                 102.639(2)
_cell_angle_gamma                97.176(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9406(13)
_cell_length_b                   15.6924(11)
_cell_length_c                   22.404(2)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.21
_cell_volume                     4732.9(7)
_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      253(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25216
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  0.6510
_exptl_absorpt_correction_T_min  0.5676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.680
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1047
_refine_ls_number_reflns         16112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0814P)^2^+8.7570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                13506
_reflns_number_total             16112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300135w_si_002_3.cif
_cod_data_source_block           6H
_cod_original_cell_volume        4733.0(7)
_cod_database_code               4329448