Nickel(I)-mediated transformations of carbon dioxide in closed synthetic cycles: reductive cleavage and coupling of CO2 generating NiICO, NiIICO3 and NiIIC2O4NiII entities
Christian Limberg; Christian Herwig; Beatrice Braun; Chem.Commun. 49 (2013) 10923–; doi:10.1039/c3cc45407j

data_7110023
_publ_section_title
;
 Nickel(I)-mediated transformations of carbon dioxide in closed synthetic
 cycles: reductive cleavage and coupling of CO2 generating NiICO, NiIICO3
 and NiIIC2O4NiII entities
;
_journal_name_full               Chem.Commun.
_journal_page_first              10923
_journal_paper_doi               10.1039/c3cc45407j
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C72 H106 N4 Ni2 O4, 4(C6 D6)'
_chemical_formula_sum            'C96 H106 D24 N4 Ni2 O4'
_chemical_formula_weight         1545.26
_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                90.00
_cell_angle_beta                 95.275(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.3703(7)
_cell_length_b                   22.7046(6)
_cell_length_c                   10.8435(4)
_cell_measurement_reflns_used    26222
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.09
_cell_volume                     4258.4(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'PLATON, 1990'
_computing_publication_material  'PLATON, 1990'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'STOE IPDS2theta'
_diffrn_measurement_method       'rotation method'
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30295
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.84
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_correction_T_min  0.8577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Spek, 2003'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                7077
_reflns_number_total             8989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45407j.txt
_cod_data_source_block           bh326wh1
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7110023