Secrets of Solid State and Aqueous Solution Structures of [Ni(tmdta)](2-).
Meier, Roland; Platas-Iglesias, Carlos; Heinemann, Frank W.; Linti, Gerald; Schulte, Jürgen; Srivastava, Sunil K.; Inorganic chemistry 53 (2014) 6684–6697; doi:10.1021/ic5004325

data_4338820
_publ_section_title
;
 Secrets of Solid State and Aqueous Solution Structures of
 [Ni(tmdta)](2-).
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6684
_journal_page_last               6697
_journal_paper_doi               10.1021/ic5004325
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C11 H14 N2 Ni O8, 2(C H6 N3), 6(O)'
_chemical_formula_sum            'C13 H38 N8 Ni O14'
_chemical_formula_weight         589.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.00
_cell_angle_beta                 93.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.832(4)
_cell_length_b                   15.174(3)
_cell_length_c                   8.4085(17)
_cell_measurement_temperature    200(2)
_cell_volume                     2653.5(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1149
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16558
_diffrn_reflns_theta_full        24.03
_diffrn_reflns_theta_max         24.03
_diffrn_reflns_theta_min         1.66
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'STOE IPDS'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.704
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.747
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.747
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.1171
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3010
_refine_ls_wR_factor_ref         0.3077
_reflns_number_gt                2494
_reflns_number_total             4150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5004325_si_003.cif
_cod_data_source_block           {C(NH2)3}2-Ni(tmdta)]-6H2O-1b
_cod_depositor_comments
'Adding full bibliography for 4338819--4338821.cif.'
_cod_original_cell_volume        2653.6(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4338820