Bis(tetraethylammonium) bis(dimethylformamide)tetrakis(μ-<i>N</i>,2-dioxidobenzene-1-carboximidato)pentacopper(II)
Herring, Jacob; Zeller, Matthias; Zaleski, Curtis M.; Acta Crystallographica Section E 67 (2011) m419–m420; doi:10.1107/S1600536811007975

data_2229730
_publ_section_title
;
 Bis(tetraethylammonium)
 bis(dimethylformamide)tetrakis(\m-<i>N</i>,2-dioxidobenzene-1-carboximidato)pentacopper(II)
;
_journal_coeditor_code           JJ2076
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m419
_journal_page_last               m420
_journal_paper_doi               10.1107/S1600536811007975
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'(C8 H20 N)2 [Cu5 (C7 H4 N O3)4 (C3 H7 N O)2]'
_chemical_formula_moiety         '2(C8 H20 N +), C34 H30 Cu5 N6 O14 2-)'
_chemical_formula_sum            'C50 H70 Cu5 N8 O14'
_chemical_formula_weight         1325.74
_chemical_name_systematic
;
Bis(tetraethylammonium) bis(dimethylformamide)tetrakis(\m-<i>N</i>,2-\
dioxidobenzene-1-carboximidato)pentacopper(II)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.641(3)
_cell_length_b                   13.616(2)
_cell_length_c                   23.238(4)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.44
_cell_volume                     5265.4(15)
_computing_cell_refinement       'APEX2 (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'APEX2 (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51635
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         31.43
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(APEX2; Bruker, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2732
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8316
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.2598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                6387
_reflns_number_total             8316
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jj2076.cif
_cod_data_source_block           I
_cod_database_code               2229730
_cod_database_fobs_code          2229730