Crystal structure of [bis(diethylenetriamine-N1,N2,N3)]-(m-oxalato-O1,O2:O1',O2')-(dimethanol-O)dinickel(II) diperchlorate, [Ni2(C4H13N3)2(C2O4)(CH3OH)2](ClO4)2
Hong Qiang; Yong Hou; Zhi-Yun Dong; Feng-Mei Nie; Zeitschrift für Kristallographie - New Crystal Structures 225 (2010) 447–; doi:

data_8102724
_publ_section_title
;
 Crystal structure of
 [bis(diethylenetriamine-N1,N2,N3)]-(m-oxalato-O1,O2:O1',O2')-(dimethanol-O)dinickel(II)
 diperchlorate, [Ni2(C4H13N3)2(C2O4)(CH3OH)2](ClO4)2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              447
_journal_volume                  225
_journal_year                    2010
_chemical_formula_sum            'C12 H34 Cl2 N6 Ni2 O14'
_chemical_formula_weight         674.77
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.6220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.12390(10)
_cell_length_b                   13.1635(2)
_cell_length_c                   14.2200(2)
_cell_measurement_temperature    273(2)
_cell_volume                     1318.42(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11888
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    1.703
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_refine_diff_density_max         1.253
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          3.170
_refine_ls_shift/su_mean         0.190
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+1.4869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1753
_reflns_number_gt                2681
_reflns_number_total             3236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3009.cff
_cod_data_source_block           0701
_cod_database_code               8102724