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_4303421
_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         'C28 H34 N4 Ni2 O6, 1.5 ( C H4 O), H2 O, 2 O'
_chemical_formula_sum            'C29.5 H42 N4 Ni2 O10.5'
_chemical_formula_weight         738.06
_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                106.232(2)
_cell_angle_beta                 91.008(2)
_cell_angle_gamma                97.590(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5932(16)
_cell_length_b                   12.1572(17)
_cell_length_c                   13.0326(18)
_cell_measurement_reflns_used    7557
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      56.45
_cell_measurement_theta_min      4.63
_cell_volume                     1745.3(4)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1993)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'omega/phi 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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17613
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  0.8385
_exptl_absorpt_correction_T_min  0.7259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0584P)^2^+3.6515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                4897
_reflns_number_total             6163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9014916_si_001_2.cif
_cod_data_source_block           5.3H2O.1.5MeOH
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_formula_sum        'C29.50 H42 N4 Ni2 O10.5'
_cod_database_code               4303421