Tetraaqua(1,10-phenanthroline)nickel(II) 3,6-dicarboxybicyclo[2.2.2]oct-7-ene-2,5-dicarboxylate
Liu, Yun-Yu; Wang, Tian-Hui; Wang, Zhi-Hao; Zhuo, Yu-Jiang; Li, Xing-Qi; Acta Crystallographica Section E 65 (2009) m978–; doi:10.1107/S1600536809028190

data_2222653
_publ_section_title
;
 Tetraaqua(1,10-phenanthroline)nickel(II)
 3,6-dicarboxybicyclo[2.2.2]oct-7-ene-2,5-dicarboxylate
;
_journal_coeditor_code           CV2585
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m978
_journal_paper_doi               10.1107/S1600536809028190
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C12 H8 N2) (H2 O)4] (C12 H10 O8)'
_chemical_formula_moiety         'C12 H16 N2 Ni O4 2+, C12 H10 O8 2-'
_chemical_formula_sum            'C24 H26 N2 Ni O12'
_chemical_formula_weight         593.18
_chemical_name_systematic
;
Tetraaqua(1,10-phenanthroline)nickel(II)
3,6-dicarboxybicyclo[2.2.2]oct-7-ene-2,5-dicarboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.000
_cell_angle_beta                 91.549(7)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   7.446(5)
_cell_length_b                   13.583(6)
_cell_length_c                   22.982(9)
_cell_measurement_reflns_used    5636
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      3.0
_cell_volume                     2324(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL-Plus (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX CCD 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     0.71069
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14211
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.472
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5636
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0737P)^2^+0.0226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                4321
_reflns_number_total             5636
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2585.cif
_cod_data_source_block           I
_cod_original_cell_volume        2323.5(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2222653
_cod_database_fobs_code          2222653