A Trinuclear Nickel(II) Enediolate Complex: Synthesis, Characterization, and O2 Reactivity
Katarzyna Rudzka; Atta M. Arif; Lisa M. Berreau; Inorganic Chemistry 47 (2008) 10832–10840; doi:10.1021/ic800947z

data_4306017
_publ_section_title
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A Trinuclear Nickel(II) Enediolate Complex: Synthesis, Characterization,
and O2 Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10832
_journal_page_last               10840
_journal_paper_doi               10.1021/ic800947z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
'C100 H94 N10 Ni3 O6,2(Cl O4),3(C2 H3 N),2(C4 H10 O)'
_chemical_formula_sum            'C114 H123 Cl2 N13 Ni3 O16'
_chemical_formula_weight         2178.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.160(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.4466(8)
_cell_length_b                   18.6303(7)
_cell_length_c                   23.8127(7)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.018
_cell_volume                     10782.8(6)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi and 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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17358
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.9506
_exptl_absorpt_correction_T_min  0.8669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long needle'
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         9891
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0485P)^2^+22.8547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                6130
_reflns_number_total             9891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800947z_si_002_1.cif
_cod_data_source_block           usu142
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4306017