Trinuclear Nickel Complexes with Metal-Arene Interactions Supported by Tris- and Bis(phosphinoaryl)benzene Frameworks.
Suseno, Sandy; Horak, Kyle T.; Day, Michael W.; Agapie, Theodor; Organometallics 32 (2013) 6883–6886; doi:10.1021/om400976x

data_4089626
_publ_section_title
;
 Trinuclear Nickel Complexes with Metal-Arene Interactions Supported by
 Tris- and Bis(phosphinoaryl)benzene Frameworks.
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6883
_journal_page_last               6886
_journal_paper_doi               10.1021/om400976x
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C34 H40 Ni3 O4 P2'
_chemical_formula_sum            'C34 H40 Ni3 O4 P2'
_chemical_formula_weight         750.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2747(6)
_cell_length_b                   14.3889(6)
_cell_length_c                   17.0160(7)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.32
_cell_measurement_theta_min      2.39
_cell_volume                     3250.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39803
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.240
_diffrn_reflns_theta_min         1.853
_exptl_absorpt_coefficient_mu    1.855
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          .94
_exptl_crystal_size_mid          .8
_exptl_crystal_size_min          0.7
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
; 
 Flack x determined using 5204 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         15869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                13142
_reflns_number_total             15869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            kth17.cif
_cod_data_source_block           kth17
_cod_database_code               4089626
_shelxl_version_number           2013-3
_shelx_res_checksum              48666
_shelx_hkl_checksum              63538