Crystal structure of poly[{aqua(1,10-phenanthroline-k^2^N,N')nickel (II)}-μ-(dihydrogen-benzene-1,2,4,5-tetracarboxylate)-k^3^O:O':O''], Ni(C10H4O8)(C12H8N2)(H2O)
J.-C. Lee; H. Takahashi; Y. Matsui; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 489–490; doi:

data_8101837
_publ_section_title
;
Crystal structure of poly[{aqua(1,10-phenanthroline-k^2^N,N')nickel
(II)}-\m-(dihydrogen-benzene-1,2,4,5-tetracarboxylate)-k^3^O:O':O''], 
Ni(C10H4O8)(C12H8N2)(H2O)
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              489
_journal_page_last               490
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety         'C22 H14 N2 Ni O9 '
_chemical_formula_sum            'C22 H14 N2 Ni O9'
_chemical_formula_weight         509.06
_chemical_name_systematic
; 
poly[[aqua(1,10-phenanthroline-\k^2^N,N')nickel(II)]-
\m-(dihydrogen-benzene-1,2,4,5-tetracarboxylato)-\k^3^O^1^:O^2^:O^3^]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                87.11(2)
_cell_angle_beta                 72.38(2)
_cell_angle_gamma                64.96(2)
_cell_formula_units_Z            2
_cell_length_a                   9.589(5)
_cell_length_b                   10.144(7)
_cell_length_c                   11.312(5)
_cell_measurement_reflns_used    9100
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     946.3(9)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  CrystalStructure
_computing_structure_refinement  'CRYSTALS (Watkin et al., 1996)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9906
_diffrn_measured_fraction_theta_max 0.9906
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9392
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Higashi, T. (1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.78
_refine_diff_density_min         -0.74
_refine_ls_extinction_coef       129(4)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.8459
_refine_ls_number_parameters     308
_refine_ls_number_reflns         3900
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.000173
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
W = [1-(deltaF/6*sigmaF)^2^]^2^/[937*T~0~(x)+138*T~1~(x)+822*T~2~(x)
+265*T~3~(x)], where T~i~ are Chebychev polynomials and x = Fc/Fmax 
(Watkin, 1994 / Prince, 1982)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0863
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0854
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3900
_reflns_number_total             4302
_reflns_threshold_expression     I>3sigma(I)
_oxford_refine_ls_scale          4.21(6)
_cod_data_source_file            1267-1611.cff
_cod_data_source_block           '_No39'
_cod_original_cell_volume        946.4(9)
_cod_original_formula_sum        'C22 H14 N2 Ni O9 '
_cod_database_code               8101837