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_4303423
_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
'C58 H66 N8 Ni4 O12, 2(C H4 O), 2 (H2 O), 2.75( O)'
_chemical_formula_sum            'C60 H78 N8 Ni4 O18.75'
_chemical_formula_weight         1446.14
_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
_cell_angle_beta                 109.876(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.567(6)
_cell_length_b                   15.566(5)
_cell_length_c                   24.071(7)
_cell_measurement_reflns_used    1018
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.985
_cell_measurement_theta_min      2.675
_cell_volume                     6542(4)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker CCD SMART1000'
_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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            95255
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        'not significant'
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  0.8489
_exptl_absorpt_correction_T_min  0.6121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2006)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         11840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0094P)^2^+1.8723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                9273
_reflns_number_total             11840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9014916_si_001_4.cif
_cod_data_source_block           7.4.75H2O.2MeOH
_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        6542(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4303423