μ-Oxalato-κ^4^<i>O</i>^1^,<i>O</i>^2^:O^1'^,<i>O</i>^2'^-bis[aqua(diethylenetriamine-κ^3^<i>N</i>)nickel(II)] bis(tetraphenylborate)
Callejo, Lorena M.; Muga, Iñaki; Vitoria, Pablo; Reinoso, Santiago; Román, Pascual; Gutiérrez-Zorrilla, Juan M.; Acta Crystallographica Section E 59 (2003) m684–m686; doi:10.1107/S1600536803016362

data_2202638
_publ_section_title
;\m-Oxalato-\k^4^<i>O</i>^1^,<i>O</i>^2^:O^1'^,<i>O</i>^2'^-bis[aqua(diethylenetriamine-\k^3^<i>N</i>)nickel(II)]
 bis(tetraphenylborate)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m684
_journal_page_last               m686
_journal_paper_doi               10.1107/S1600536803016362
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'[Ni2 (C2 O4) (C4 H13 N3)2 (H2 O)2] (C24 H20 B1)2'
_chemical_formula_moiety         'C10 H30 N6 Ni2 O6 2+, 2C24 H20 B1 1-'
_chemical_formula_sum            'C58 H70 B2 N6 Ni2 O6'
_chemical_formula_weight         1086.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8500(10)
_cell_length_b                   19.576(3)
_cell_length_c                   13.020(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.26
_cell_measurement_theta_min      9.6
_cell_volume                     2734.9(6)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2002)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99.2 (Beurskens et al., 1999)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8287
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.498
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.103
_refine_ls_R_factor_gt           0.0451
_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^)+(0.057P)^2^+0.7675P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.104
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                4921
_reflns_number_total             7975
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl6050.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2202638
_cod_database_fobs_code          2202638