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_4102394
_publ_section_title
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 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         'C30 H40 Ni P2'
_chemical_formula_sum            'C30 H40 Ni P2'
_chemical_formula_weight         521.27
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5770(3)
_cell_length_b                   14.8684(5)
_cell_length_c                   21.6483(7)
_cell_measurement_reflns_used    9171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.90
_cell_measurement_theta_min      2.33
_cell_volume                     2760.73(16)
_computing_cell_refinement       'Bruker SAINT-Plus v7.34A'
_computing_data_collection       'Bruker APEX2 v2.1-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.34A'
_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 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 12 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  0.0956
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            64242
_diffrn_reflns_theta_full        35.07
_diffrn_reflns_theta_max         35.07
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.9212
_exptl_absorpt_correction_T_min  0.7532
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.311
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     458
_refine_ls_number_reflns         10653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.311
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_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          0.0568
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                9264
_reflns_number_total             10653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja101699a_si_003.cif
_cod_data_source_block           av08
_cod_depositor_comments
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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 'Difference Fourier map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4102394