Binuclear Complexes Containing a Methylnickel Moiety: Relevance to Organonickel Intermediates in Acetyl Coenzyme A Synthase Catalysis
William G. Dougherty; Krishnan Rangan; Molly J. O'Hagan; Glenn P. A. Yap; Charles G. Riordan; Journal of the American Chemical Society 130 (2008) 13510–13511; doi:10.1021/ja803795k

data_4108471
_publ_section_title
;
 Binuclear Complexes Containing a Methylnickel Moiety: Relevance to
 Organonickel Intermediates in Acetyl Coenzyme A Synthase Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13510
_journal_page_last               13511
_journal_paper_doi               10.1021/ja803795k
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C48 H50 N2 Ni2 O3 P2 S2'
_chemical_formula_weight         946.38
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_beta                 107.046(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.029(3)
_cell_length_b                   19.121(2)
_cell_length_c                   17.573(2)
_cell_measurement_reflns_used    1007
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.83
_cell_measurement_theta_min      2.45
_cell_volume                     4506.8(12)
_computing_cell_refinement       'SHELXTL, Sheldrick (2001)'
_computing_data_collection       'SMART, Bruker (2002)'
_computing_data_reduction        'SHELXTL, Sheldrick (2001)'
_computing_molecular_graphics    'SHELXTL, Sheldrick (2001)'
_computing_publication_material  'SHELXTL, Sheldrick (2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37170
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.9029
_exptl_absorpt_correction_T_min  0.8186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
; Void space analysis consistent with 4 THF molecules per unit cell.
  PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         10272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0557P)^2^+0.0778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                8490
_reflns_number_total             10272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja803795k_si_001.cif
_cod_data_source_block           char103s
_cod_original_cell_volume        4506.9(11)
_cod_database_code               4108471