A novel tridentate coordination mode for the carbonatonickel system exhibited in an unusual hexanuclear nickel(ii) μ3-carbonato-bridged complex
Anderson, James C.; Blake, Alexander J.; Moreno, Rafael Bou; Raynel, Guillaume; van Slageren, Joris; Dalton Transactions  (2009) 9153–; doi:10.1039/b912612k

data_7002607
_publ_section_title
;
 A novel tridentate coordination mode for the carbonatonickel system
 exhibited in an unusual hexanuclear nickel(ii) \m3-carbonato-bridged
 complex
;
_journal_issue                   42
_journal_name_full               'Dalton Transactions'
_journal_page_first              9153
_journal_paper_doi               10.1039/b912612k
_journal_year                    2009
_chemical_formula_moiety         'C40 H120 N12 Ni6 O24, C H2 Cl2, 4(Cl)'
_chemical_formula_sum            'C41 H122 Cl6 N12 Ni6 O24'
_chemical_formula_weight         1733.46
_chemical_name_systematic
;
?
;
_space_group_IT_number           218
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_space_group_name_H-M   'P -4 3 n'
_atom_sites_solution_hydrogens
'water H atoms not located; others placed geometrically'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF outout'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.1334(2)
_cell_length_b                   26.1334(2)
_cell_length_c                   26.1334(2)
_cell_measurement_reflns_used    22915
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.2
_cell_volume                     17847.9(2)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            110668
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_T_max  0.472
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Bruker SHELXTL; Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             7320
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.45
_refine_diff_density_rms         0.09
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         6827
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.053P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                6185
_reflns_number_total             6827
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b912612k.txt
_cod_data_source_block           ninall
_cod_original_cell_volume        17848(2)
_cod_database_code               7002607