Tris(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')nickel(II) bis(2,4,5-tricarboxybenzoate) monohydrate
Zhong, Kai-Long; Ni, Chao; Qian, Ming-Yi; Acta Crystallographica Section E 67 (2011) m1814–m1815; doi:10.1107/S1600536811048914

data_2232563
_publ_section_title
;
 Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')nickel(II)
 bis(2,4,5-tricarboxybenzoate) monohydrate
;
_journal_coeditor_code           BQ2318
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1814
_journal_page_last               m1815
_journal_paper_doi               10.1107/S1600536811048914
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C12 H8 N2)3] (C10 H5 O8)2, H2 O'
_chemical_formula_moiety         'C36 H24 N6 Ni 2+, 2(C10 H5 O8 -), H2 O'
_chemical_formula_sum            'C56 H36 N6 Ni O17'
_chemical_formula_weight         1123.62
_chemical_name_systematic
;
Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')nickel(II)
bis(2,4,5-tricarboxybenzoate) monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 116.271(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.2009(11)
_cell_length_b                   14.1546(5)
_cell_length_c                   15.8347(7)
_cell_measurement_reflns_used    4069
_cell_measurement_temperature    295.15
_cell_measurement_theta_max      29.2225
_cell_measurement_theta_min      2.8157
_cell_volume                     4864.0(4)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295.15
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur Sapphire3 Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0788
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12270
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.8680
_exptl_absorpt_correction_T_min  0.8294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSPACK; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.418
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4977
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0092P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                3050
_reflns_number_total             4977
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bq2318.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2232563
_cod_database_fobs_code          2232563