Building Metallacrown Topology around a Discrete [M3(μ3-O)] (M = Ni(II) and Pd(II)) Core Using Oximato Oxygen Linkers: Synthesis, Structures, and Spectroscopic Characterization of a New Family of Compounds with an Inverse-9-MC-3 Motif
Anandalok Audhya; Kisholoy Bhattacharya; Manoranjan Maity; Muktimoy Chaudhury; Inorganic Chemistry 49 (2010) 5009–5015; doi:10.1021/ic100179q

data_4315599
_publ_section_title
;
 Building Metallacrown Topology around a Discrete [M3(\m3-O)] (M = Ni(II)
 and Pd(II)) Core Using Oximato Oxygen Linkers: Synthesis, Structures, and
 Spectroscopic Characterization of a New Family of Compounds with an
 Inverse-9-MC-3 Motif
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5009
_journal_page_last               5015
_journal_paper_doi               10.1021/ic100179q
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C24 H45 Cl N6 Ni3 O8'
_chemical_formula_weight         757.24
_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                76.802(3)
_cell_angle_beta                 76.656(3)
_cell_angle_gamma                78.646(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7618(10)
_cell_length_b                   12.3220(11)
_cell_length_c                   12.4946(10)
_cell_measurement_temperature    298(2)
_cell_volume                     1695.4(3)
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_collection       'BRUKER APEX II'
_computing_data_reduction        'BRUKER APEX II'
_computing_molecular_graphics    'MERCURY 2.2, PLATON-97'
_computing_publication_material  'MERCURY 2.2, PLATON-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_measurement_method       OMEGA-SCAN
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            16158
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_T_max  0.7641
_exptl_absorpt_correction_T_min  0.5366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0449
_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^+0.3580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                4107
_reflns_number_total             6160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100179q_si_003.cif
_cod_data_source_block           Comp-2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1695.4(2)
_cod_database_code               4315599