Tris(1,10-phenanthroline)cadmium 3,3'-dicarboxy-4,4'-diazenediyldibenzoate‒4,4'-diazenediyldiphthalic acid‒methanol (1/0.5/1)
Wang, Jun; Lu, Lu; Wei-Ping, Wu; He, Xi-Yang; Tao, Wang; Acta Crystallographica Section E 67 (2011) m867–m868; doi:10.1107/S160053681102068X

data_2230606
_publ_section_title
;
 Tris(1,10-phenanthroline)cadmium
 3,3'-dicarboxy-4,4'-diazenediyldibenzoate--4,4'-diazenediyldiphthalic
 acid--methanol (1/0.5/1)
;
_journal_coeditor_code           DN2688
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m867
_journal_page_last               m868
_journal_paper_doi               10.1107/S160053681102068X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Cd (C12 H8 N2)3] (C16 H8 N2 O8), 0.5C16 H10 N2 O8, C H4 O'
_chemical_formula_moiety
'C36 H24 Cd N6 2+, C16 H8 N2 O8 2-, 0.5(C16 H10 N2 O8), C H4 O'
_chemical_formula_sum            'C61 H41 Cd N9 O13'
_chemical_formula_weight         1220.43
_chemical_name_systematic
;
Tris(1,10-phenanthroline)cadmium
3,3'-dicarboxy-4,4'--diazenediyldibenzoate--
4,4'-diazenediyldiphthalic acid--methanol (1/0.5/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.0220(10)
_cell_angle_beta                 73.4920(10)
_cell_angle_gamma                64.4390(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6902(9)
_cell_length_b                   13.7659(9)
_cell_length_c                   16.9518(11)
_cell_measurement_reflns_used    10030
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.35
_cell_volume                     2754.7(3)
_computing_cell_refinement       'APEX2 (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'APEX2 (Bruker, 2008)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997) and
Mercury (Macrae <i>et al.</i>, 2006, 2010)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
and PLATON (van der Sluis & Spek, 1990; Spek, 2003)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21086
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.49
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.9679
_exptl_absorpt_correction_T_min  0.8998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
Some residual electron density were difficult to model and therefore, the
SQUEEZE function of PLATON (Spek, 2009) was used to eliminate the contribution
of the electron density in the solvent region from the intensity data, and the
solvent-free model was employed for the final refinement.
There are two cavities cavities of 115\%A^3^ per unit cell. PLATON
estimated that each cavity contains 17 electrons which may roughly
correspond to a mixture of solvent molecule of methanol
molecule as suggested by chemical analyses.
;
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         9876
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                8170
_reflns_number_total             10030
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2688.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               2230606
_cod_database_fobs_code          2230606