The neutral cluster amminehexa-μ~2~-chlorido-μ~4~-oxido-tris(1,4,6-triazabicyclo[3.3.0]oct-4-ene)tetracopper(II)
Chiarella, Gina M.; Melgarejo, Doris Y.; Fackler Jr, John P.; Acta Crystallographica Section C 65 (2009) m228–m230; doi:10.1107/S0108270109015054

data_2017128
_publ_section_title
;The neutral cluster
 amminehexa-\m~2~-chlorido-\m~4~-oxido-tris(1,4,6-triazabicyclo[3.3.0]oct-4-ene)tetracopper(II)
;
_journal_coeditor_code           FA3183
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m228
_journal_page_last               m230
_journal_paper_doi               10.1107/S0108270109015054
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Cu4 Cl6 O (C5 H9 N3)3 (N H3)]'
_chemical_formula_moiety         'C15 H30 Cl6 Cu4 N10 O'
_chemical_formula_sum            'C15 H30 Cl6 Cu4 N10 O'
_chemical_formula_weight         833.35
_chemical_name_systematic
;
amminehexa-\m~2~-chlorido-\m~4~-oxido-tris(1,4,6-triazabicyclo[3.3.0]oct-4-
ene)tetracopper(II)
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_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                   17.548(9)
_cell_length_b                   17.548(9)
_cell_length_c                   7.898(4)
_cell_measurement_reflns_used    2221
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.32
_cell_volume                     2106.2(19)
_computing_cell_refinement       'APEX2 (Bruker--Nonius, 2008)'
_computing_data_collection       'APEX2 (Bruker--Nonius, 2008)'
_computing_data_reduction        'APEX2 (Bruker--Nonius, 2008)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6295
_diffrn_reflns_theta_full        26.70
_diffrn_reflns_theta_max         26.70
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.590
_exptl_absorpt_correction_T_max  0.8107
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.307
_refine_ls_abs_structure_details 'Flack (1983), 983 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.019(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1972
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0628
_reflns_number_gt                1772
_reflns_number_total             1972
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3183.cif
_cod_data_source_block           I
_cod_original_cell_volume        2106.2(17)
_cod_original_sg_symbol_Hall     R3
_cod_original_sg_symbol_H-M      R3
_cod_database_code               2017128
_cod_database_fobs_code          2017128