CO oxidation at nickel centres by N2O or O2 to yield a novel hexanuclear carbonate
Bettina Horn; Christian Limberg; Christian Herwig; Michael Feist; Stefan Mebs; Chem.Commun. 48 (2012) 8243–; doi:10.1039/c2cc33846g

data_7108156
_publ_section_title
;
 CO oxidation at nickel centres by N2O or O2 to yield a novel hexanuclear
 carbonate
;
_journal_name_full               Chem.Commun.
_journal_page_first              8243
_journal_paper_doi               10.1039/c2cc33846g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C216 H318 K6 N12 Ni6 O18, 5(C6 H14)'
_chemical_formula_sum            'C246 H388 K6 N12 Ni6 O18'
_chemical_formula_weight         4388.54
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.00
_cell_angle_beta                 95.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.165(3)
_cell_length_b                   21.255(4)
_cell_length_c                   41.304(8)
_cell_measurement_reflns_used    140596
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      3.11
_cell_volume                     14125(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        XPREP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      ' 724 frames, detector distance = 120 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            139094
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.11
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           45
_diffrn_source_power             2.25
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.8705
_exptl_absorpt_correction_T_min  0.6853
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XPREP '
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4748
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;

;
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1514
_refine_ls_number_reflns         25957
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0741
_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^)+(0.1338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1962
_refine_ls_wR_factor_ref         0.2155
_reflns_number_gt                17566
_reflns_number_total             25957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33846g.txt
_cod_data_source_block           c:2012_bh66
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7108156