Tris(1,10-phenanthroline-5,6-dione-κ^2^<i>N</i>,<i>N</i>')zinc bis(perchlorate) acetonitrile monosolvate
Zhao, Jing; Zhang, Heng; Zhang, Zhaozhi; Zhao, Haiyan; Zhu, Guoyi; Acta Crystallographica Section E 67 (2011) m1422–m1423; doi:10.1107/S1600536811037081

data_2231929
_publ_section_title
;
 Tris(1,10-phenanthroline-5,6-dione-\k^2^<i>N</i>,<i>N</i>')zinc
 bis(perchlorate) acetonitrile monosolvate
;
_journal_coeditor_code           HY2471
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1422
_journal_page_last               m1423
_journal_paper_doi               10.1107/S1600536811037081
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Zn (C12 H6 N2 O2)3] (Cl O4)2, C2 H3 N'
_chemical_formula_moiety         'C36 H18 N6 O6 Zn 2+, 2(Cl O4 -), C2 H3 N'
_chemical_formula_sum            'C38 H21 Cl2 N7 O14 Zn'
_chemical_formula_weight         935.91
_chemical_name_systematic
;
Tris(1,10-phenanthroline-5,6-dione-\k^2^<i>N</i>,<i>N</i>')zinc
bis(perchlorate) acetonitrile monosolvate
;
_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           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                   13.446(6)
_cell_length_b                   14.125(6)
_cell_length_c                   20.483(8)
_cell_measurement_reflns_used    5261
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.49
_cell_measurement_theta_min      2.32
_cell_volume                     3890(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1108
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23200
_diffrn_reflns_theta_full        28.56
_diffrn_reflns_theta_max         28.56
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.9050
_exptl_absorpt_correction_T_min  0.7847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.392
_refine_ls_abs_structure_details 'Flack (1983), 4095 Friedel pairs'
_refine_ls_abs_structure_Flack   0.12(2)
_refine_ls_extinction_coef       0.0031(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9569
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0748
_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^)+(0.1231P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.2201
_reflns_number_gt                5533
_reflns_number_total             9569
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2471.cif
_cod_data_source_block           I
_cod_database_code               2231929
_cod_database_fobs_code          2231929