Bis(triethanolamine-κ^3^<i>N,O,O</i>')nickel(II) squarate
Yeşilel, Okan Zafer; Bulut, Ahmet; Uçar, İbrahim; İçbudak, Hasan; Ölmez, Halis; Büyükgüngör, Orhan; Acta Crystallographica Section E 60 (2004) m228–m230; doi:10.1107/S1600536804001503

data_2203208
_publ_section_title
;
 Bis(triethanolamine-\k^3^<i>N,O,O</i>')nickel(II) squarate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m228
_journal_page_last               m230
_journal_paper_doi               10.1107/S1600536804001503
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (C6 H15 N O3)2] (C4 O4)'
_chemical_formula_moiety         'C12 H30 N2 Ni O6 2+, C4 O4 2-'
_chemical_formula_sum            'C16 H30 N2 Ni O10'
_chemical_formula_weight         469.13
_chemical_name_systematic        ?
_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                102.551(7)
_cell_angle_beta                 110.398(7)
_cell_angle_gamma                99.698(7)
_cell_formula_units_Z            1
_cell_length_a                   7.5058(7)
_cell_length_b                   8.5766(8)
_cell_length_c                   8.9156(8)
_cell_measurement_reflns_used    15818
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.11
_cell_measurement_theta_min      0.00
_cell_volume                     506.04(9)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  ' Stoe IPDS-2'
_diffrn_measurement_method       '\w rotation'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6624
_diffrn_reflns_theta_full        32.17
_diffrn_reflns_theta_max         32.17
_diffrn_reflns_theta_min         2.52
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.7716
_exptl_absorpt_correction_T_min  0.5162
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 2002)'
_exptl_crystal_colour            Violet
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             248
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.573
_refine_ls_extinction_coef       0.108(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0472P)^2^+0.0971P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                3346
_reflns_number_total             3549
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6286.cif
_cod_data_source_block           I
_cod_database_code               2203208
_cod_database_fobs_code          2203208