Tris(1,10-phenanthroline-5,6-dione-κ^2^<i>N</i>,<i>N</i>')copper(II) bis(perchlorate) 4.5-hydrate
Khalaji, Aliakbar Dehno; Slawin, Alexandra M. Z.; Woollins, J. Derek; Acta Crystallographica Section E 63 (2007) m2848–m2848; doi:10.1107/S1600536807052348

data_2215787
_publ_section_title
;
 Tris(1,10-phenanthroline-5,6-dione-\k^2^<i>N</i>,<i>N</i>')copper(II)
 bis(perchlorate) 4.5-hydrate
;
_journal_coeditor_code           BR2056
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2848
_journal_page_last               m2848
_journal_paper_doi               10.1107/S1600536807052348
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu (C12 H6 N2 O2)3] (Cl O4)2 , 4.5H2 O'
_chemical_formula_moiety         'C36 H18 Cu N6 O6 2+ , 2Cl O4 - , 4.5H2 O'
_chemical_formula_sum            'C36 H27 Cl2 Cu N6 O18.5'
_chemical_formula_weight         974.08
_chemical_name_systematic
;
Tris(1,10-phenanthroline-5,6-dione-\k^2^N,N')copper(II) bis(perchlorate)
4.5-hydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.136(2)
_cell_length_b                   14.071(2)
_cell_length_c                   20.636(3)
_cell_measurement_reflns_used    12591
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.7539
_cell_measurement_theta_min      1.5502
_cell_volume                     3814.3(10)
_computing_cell_refinement       'CrystalClear (Rigaku, 2004)'
_computing_data_collection       'CrystalClear (Rigaku, 2004)'
_computing_data_reduction        'CrystalClear (Rigaku, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2003)'
_computing_publication_material  'SHELXTL (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24980
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.1000
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.445
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.517(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         6940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.066P)^2^+2.3835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                6206
_reflns_number_total             6940
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2056.cif
_cod_data_source_block           I
_cod_original_cell_volume        3814.2(10)
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_original_formula_sum        'C36 H27 Cl2 Cu N6 O18.50'
_cod_database_code               2215787
_cod_database_fobs_code          2215787