Synthesis, Characterization, and Reactivity of Nickel Hydride Complexes Containing 2,6-C6H3(CH2PR2)2(R = tBu,cHex, and iPr) Pincer Ligands
Boro, Brian J.; Duesler, Eileen N.; Goldberg, Karen I.; Kemp, Richard A.; Inorganic Chemistry 48 (2009) 5081–5087; doi:10.1021/ic8020194

data_4338609
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of Nickel Hydride Complexes
 Containing 2,6-C6H3(CH2PR2)2(R = tBu,cHex, and iPr) Pincer Ligands
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_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5081
_journal_page_last               5087
_journal_paper_doi               10.1021/ic8020194
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C32 H52 Ni P2'
_chemical_formula_sum            'C32 H52 Ni P2'
_chemical_formula_weight         557.39
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   19.960(2)
_cell_length_b                   26.455(3)
_cell_length_c                   27.789(3)
_cell_measurement_reflns_used    9599
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      2.51
_cell_volume                     14674(3)
_computing_cell_refinement       'APEX2, Bruker AXS Inc.'
_computing_data_collection       'APEX2, Bruker AXS Inc.'
_computing_data_reduction        'APEX2, Bruker AXS Inc.'
_computing_molecular_graphics    'Diamond 3.1 (Brandenburg, 1999)'
_computing_structure_refinement  'Bruker SHELXTL XS (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      228(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0000
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_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12268
_diffrn_reflns_theta_full        31.55
_diffrn_reflns_theta_max         31.55
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.8116
_exptl_absorpt_correction_T_min  0.7406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker,SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cut
_exptl_crystal_F_000             4832
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.34
_platon_squeeze_details
;
;
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         12268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+5.9735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1308
_reflns_number_gt                8533
_reflns_number_total             12268
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8020194_si_001.cif
_cod_data_source_block           rkbb7bs_Fig_2b
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
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_cod_original_sg_symbol_H-M      Ccca
_cod_database_code               4338609