High-Spin M2+Carboxylate Triangles from the Microwave
Milios, Constantinos J.; Prescimone, Alessandro; Sanchez-Benitez, J.; Parsons, Simon; Murrie, Mark; Brechin, Euan K.; Inorganic Chemistry 45 (2006) 7053–7055; doi:10.1021/ic061035o

data_4332890
_publ_section_title
;
 High-Spin M2+Carboxylate Triangles from the Microwave
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7053
_journal_page_last               7055
_journal_paper_doi               10.1021/ic061035o
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source        'C. Milios'
_chemical_formula_moiety         '[Ni3(py)5(acetate)3(azide)3]'
_chemical_formula_sum            'C31 H34 N14 Ni3 O6'
_chemical_formula_weight         874.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_date             06-02-07
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                90
_cell_angle_beta                 100.352(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5737(3)
_cell_length_b                   13.7069(4)
_cell_length_c                   25.3967(7)
_cell_measurement_reflns_used    4868
_cell_measurement_temperature    150
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     3620.90(18)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker SMART Apex CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            37308
_diffrn_reflns_theta_full        28.365
_diffrn_reflns_theta_max         30.500
_diffrn_reflns_theta_min         1.981
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.608
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS version 2004/1'
_exptl_crystal_colour            turquoise
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_recrystallization_method
;
Recrystallisation by layering of diethyl ether with a pyridine and 
methanol solution.
;
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.7201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.000242
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1797
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1797
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                5893
_reflns_number_total             10312
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.21754(17)
_cod_data_source_file            ic061035osup1.cif
_cod_data_source_block           eb6015
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4332890