Discovering the Complex Chemistry of a Simple NiII/H3L System: Magnetostructural Characterization and DFT Calculations of Di- and Polynuclear Nickel(II) Compounds
Matilde Fondo; Noelia Ocampo; Ana M. García-Deibe; Eliseo Ruíz; Javier Tercero; Jesús Sanmartín; Inorganic Chemistry 48 (2009) 9861–9873; doi:10.1021/ic9014916

data_4303420
_publ_section_title
;
Discovering the Complex Chemistry of a Simple NiII/H3L System:
Magnetostructural Characterization and DFT Calculations of Di- and
Polynuclear Nickel(II) Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9861
_journal_page_last               9873
_journal_paper_doi               10.1021/ic9014916
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C34 H34 N4 Ni2 O6, 1.75 (H2 O)'
_chemical_formula_sum            'C34 H37.5 N4 Ni2 O7.75'
_chemical_formula_weight         743.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 102.021(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5342(19)
_cell_length_b                   21.469(4)
_cell_length_c                   14.727(2)
_cell_measurement_reflns_used    932
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.79
_cell_volume                     3566.8(10)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_data_reduction        'BRUKER Saint'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25384
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.937499
_exptl_absorpt_correction_T_min  0.663667
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1550
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1191P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1977
_reflns_number_gt                4287
_reflns_number_total             7234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9014916_si_001_1.cif
_cod_data_source_block           4.1.75H2O
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3566.9(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C34 H37.50 N4 Ni2 O7.75'
_cod_database_code               4303420