Synthesis of Low-Valent Nickel Complexes in Aqueous Media, Mechanistic Insights, and Selected Applications
Morales-Becerril, Illán; Flores-Álamo, Marcos; Tlahuext-Aca, Adrián; Arévalo, Alma; García, Juventino J.; Organometallics 33 (2014) 6796–; doi:10.1021/om500767p

data_4084755
_publ_section_title
;
 Synthesis of Low-Valent Nickel Complexes in Aqueous Media, Mechanistic
 Insights, and Selected Applications
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6796
_journal_paper_doi               10.1021/om500767p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C28 H66 Ni2 O2 P4, 2(F6 P)'
_chemical_formula_sum            'C28 H66 F12 Ni2 O2 P6'
_chemical_formula_weight         966.04
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
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_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_c                   12.2178(4)
_cell_measurement_reflns_used    4226
_cell_measurement_temperature    105(2)
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_computing_cell_refinement
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      105(2)
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0435843
_diffrn_orient_matrix_UB_12      0.0125533
_diffrn_orient_matrix_UB_13      -0.1307268
_diffrn_orient_matrix_UB_21      0.0179532
_diffrn_orient_matrix_UB_22      -0.0701316
_diffrn_orient_matrix_UB_23      -0.0212081
_diffrn_orient_matrix_UB_31      -0.1801429
_diffrn_orient_matrix_UB_32      -0.0099811
_diffrn_orient_matrix_UB_33      -0.0153074
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_Laue_measured_fraction_full 1
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_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13910
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.102
_diffrn_reflns_theta_min         4.127
_exptl_absorpt_coefficient_mu    3.875
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.84
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3953
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+4.7025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                3121
_reflns_number_total             3953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500767p_si_002.cif
_cod_data_source_block           2b-imb089e
_cod_depositor_comments
'Adding full bibliography for 4084755--4084760.cif.'
_cod_original_cell_volume        2164.95(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4084755
_shelx_estimated_absorpt_t_min   0.432
_shelx_estimated_absorpt_t_max   0.675