Crystal structure of aqua{μ-<i>N</i>-[3-(dimethylamino)propyl]-<i>N</i>'-2-(oxidophenyl)oxamidato}(1,10-phenanthroline-5,6-dione)dicopper(II) perchlorate hemihydrate
Zhang, Xin; Li, Yan-Tuan; Wu, Zhi-Yong; Acta Crystallographica Section E 71 (2015) 667–670; doi:10.1107/S2056989015009391

data_2240772
_publ_section_title
;
 Crystal structure of
 aqua{\m-<i>N</i>-[3-(dimethylamino)propyl]-<i>N</i>'-2-(oxidophenyl)oxamidato}(1,10-phenanthroline-5,6-dione)dicopper(II)
 perchlorate hemihydrate
;
_journal_coeditor_code           XU5850
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              667
_journal_page_last               670
_journal_paper_doi               10.1107/S2056989015009391
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Cu2 (C13 H16 N3 O3) (C12 H6 N2 O2) (H2 O1)] Cl O4, 0.5H2 O'
_chemical_formula_moiety         'Cu2 C25 H24 N5 O6 +, Cl O4 -, 0.5(H2 O)'
_chemical_formula_sum            'C25 H25 Cl Cu2 N5 O10.5'
_chemical_formula_weight         726.033
_chemical_name_systematic
'Aqua{\m-<i>N</i>-[3-(dimethylamino)propyl]-<i>N</i>'-2-(oxidophenyl)oxamidato}(1,10-phenanthroline-5,6-dione)dicopper(II) perchlorate hemihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 98.1540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7430(6)
_cell_length_b                   17.3066(9)
_cell_length_c                   14.1086(8)
_cell_measurement_reflns_used    9065
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.406
_cell_measurement_theta_min      3.146
_cell_volume                     2838.3(3)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21066
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_T_max  0.9070
_exptl_absorpt_correction_T_min  0.6358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2002)
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       prism
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.475
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6432
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0369P)^2^+7.4021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                4831
_reflns_number_total             6432
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5850sup1.cf
_cod_data_source_block           I
_cod_original_formula_sum        'C25 H25 Cl Cu2 N5 O10.50'
_cod_database_code               2240772
_cod_database_fobs_code          2240772
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.905
_shelxl_version_number           199.7