Crystal structure of a binuclear nickel(II) complex constructed of 1<i>H</i>-imidazo[4,5-<i>f</i>][1,10]phenanthroline and doubly deprotonated benzene-1,3,5-tricarboxylic acid
Lv, Ying; Hao, Xiang-Rong; Acta Crystallographica Section E 71 (2015) m95–m96; doi:10.1107/S205698901500420X

data_2240513
_publ_section_title
;
 Crystal structure of a binuclear nickel(II) complex constructed of
 1<i>H</i>-imidazo[4,5-<i>f</i>][1,10]phenanthroline and doubly
 deprotonated benzene-1,3,5-tricarboxylic acid
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m95
_journal_page_last               m96
_journal_paper_doi               10.1107/S205698901500420X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ni2 (C9 H4 O6)2 (C13 H8 N4)2 (H2 O)4], 2H2 O'
_chemical_formula_moiety         'C44 H32 N8 Ni2 O16, 2(H2 O)'
_chemical_formula_sum            'C44 H36 N8 Ni2 O18'
_chemical_formula_weight         1082.22
_chemical_name_systematic
'Bis(\m-5-carboxybenzene-1,3-dicarboxylato-\k^2^<i>O</i>^1^:<i>O</i>^1'^)bis[diaqua(1<i>H</i>-imidazo[4,5-<i>f</i>][1,10]phenanthroline-\k^2^<i>N</i>^7^,<i>N</i>^8^)nickel(II)] dihydrate'
_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                82.222(5)
_cell_angle_beta                 87.729(5)
_cell_angle_gamma                73.117(5)
_cell_formula_units_Z            1
_cell_length_a                   8.581(5)
_cell_length_b                   9.032(5)
_cell_length_c                   14.278(5)
_cell_measurement_reflns_used    2586
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      3.58
_cell_volume                     1049.2(9)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5594
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.8670
_exptl_absorpt_correction_T_min  0.8054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                3050
_reflns_number_total             3851
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zp2016sup1.cf
_cod_data_source_block           I
_cod_database_code               2240513
_cod_database_fobs_code          2240513