Synthesis and C-C Coupling Reactivity of a Dinuclear NiI-NiI Complex Supported by a Terphenyl Diphosphine
Alexandra Velian; Sibo Lin; Alexander J. M. Miller; Michael W. Day; Theodor Agapie; Journal of the American Chemical Society 132 (2010) 6296–6297; doi:10.1021/ja101699a

data_4102396
_publ_section_title
;
 Synthesis and C-C Coupling Reactivity of a Dinuclear NiI-NiI Complex
 Supported by a Terphenyl Diphosphine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6296
_journal_page_last               6297
_journal_paper_doi               10.1021/ja101699a
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'0.80(C34 H40 Ni2 O4 P2) 0.20(C36 H40 Ni2 O6 P2)'
_chemical_formula_sum            'C34.41 H40 Ni2 O4.41 P2'
_chemical_formula_weight         703.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.794(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1846(13)
_cell_length_b                   25.477(4)
_cell_length_c                   9.4217(16)
_cell_measurement_reflns_used    1183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.10
_cell_measurement_theta_min      2.72
_cell_volume                     1694.1(5)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 5 settings'
_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  0.1165
_diffrn_reflns_av_sigmaI/netI    0.1454
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14281
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/2, Bruker-AXS, Madison, WI'
_exptl_crystal_colour            'Dichroic - orange/yellow'
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             735
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3311
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                1827
_reflns_number_total             3311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja101699a_si_005.cif
_cod_data_source_block           sbl04
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'Sigma' changed to 'sigma'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4102396