Bis{μ~3~-<i>cis</i>-<i>N</i>-(2-carboxylato-5-chlorophenyl)-<i>N</i>'-[3-(dimethylamino)propyl]oxamidato(3{-})}bis(perchlorato-κ<i>O</i>)bis(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethylenediamine)tetracopper(II)
Sun, Yanlong; Xu, Xuelian; Acta Crystallographica Section E 67 (2011) m645–m646; doi:10.1107/S1600536811014978

data_2230119
_publ_section_title
;
 Bis{\m~3~-<i>cis</i>-<i>N</i>-(2-carboxylato-5-chlorophenyl)-<i>N</i>'-[3-(dimethylamino)propyl]oxamidato(3{-})}bis(perchlorato-\k<i>O</i>)bis(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethylenediamine)tetracopper(II)
;
_journal_coeditor_code           PV2408
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m645
_journal_page_last               m646
_journal_paper_doi               10.1107/S1600536811014978
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Cu4 (C14 H15 Cl N3 O4)2 (Cl O4)2 (C6 H16 N2)2]'
_chemical_formula_moiety         'C40 H62 Cl4 Cu4 N10 O16'
_chemical_formula_sum            'C40 H62 Cl4 Cu4 N10 O16'
_chemical_formula_weight         1334.96
_chemical_name_systematic
;
Bis{\m~3~-<i>cis</i>-<i>N</i>-(2-carboxylato-5-chlorophenyl)-<i>N</i>'-
[3-(dimethylamino)propyl]oxamidato(3-)}bis(perchlorato-
\k<i>O</i>)bis(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-
tetramethylethylenediamine)tetracopper(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 113.988(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5750(13)
_cell_length_b                   16.4137(19)
_cell_length_c                   14.1080(15)
_cell_measurement_reflns_used    4604
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.741
_cell_measurement_theta_min      2.214
_cell_volume                     2660.4(5)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12993
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.853
_exptl_absorpt_correction_T_max  0.7082
_exptl_absorpt_correction_T_min  0.4638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.757
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0720P)^2^+1.0008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                3287
_reflns_number_total             4682
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2408.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2230119
_cod_database_fobs_code          2230119