Self-Assembled Organometallic Nickel Complexes as Catalysts for Selective Dimerization of Ethylene into 1-Butene
Boulens, Pierre; Pellier, Emmanuel; Jeanneau, Erwann; Reek, Joost N. H.; Olivier-Bourbigou, Hélène; Breuil, Pierre-Alain R.; Organometallics 34 (2015) 1139–; doi:10.1021/acs.organomet.5b00055

data_4087398
_publ_section_title
;
 Self-Assembled Organometallic Nickel Complexes as Catalysts for Selective
 Dimerization of Ethylene into 1-Butene
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1139
_journal_paper_doi               10.1021/acs.organomet.5b00055
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C38 H45 F3 N2 Ni1 O2 P2 S1'
_chemical_formula_sum            'C38 H45 F3 N2 Ni O2 P2 S'
_chemical_formula_weight         771.50
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.811(2)
_cell_length_b                   18.315(2)
_cell_length_c                   18.962(3)
_cell_measurement_reflns_used    3983
_cell_measurement_temperature    150
_cell_measurement_theta_max      67.0680
_cell_measurement_theta_min      4.5300
_cell_volume                     3741.9(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.791
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.130
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11721
_diffrn_reflns_theta_full        66.851
_diffrn_reflns_theta_max         90.000
_diffrn_reflns_theta_min         3.360
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.500
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.59
_refine_diff_density_min         -1.44
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6794
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          0.0001173
_refine_ls_shift/su_mean         0.0000082
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 269. 327. 156. 18.8 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2103
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.2103
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                4438
_reflns_number_total             6515
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.61
_oxford_diffrn_Wilson_scale      1.21
_oxford_refine_ls_r_factor_ref   0.1438
_oxford_refine_ls_scale          1.113(6)
_oxford_reflns_number_all        6794
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om5b00055_si_003.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C38 H45 F3 N2 Ni1 O2 P2 S1'
_cod_database_code               4087398
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE N   (   2,X'S) H   (   2,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  52,X'S) H   (  53,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) H   (  63,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  30,X'S) H   ( 303,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 413,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 442,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 462,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 472,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 482,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = N(20) TO S(21) 
U(IJ)'S  0.0, 0.010000 = C(35) TO C(40) 
U(IJ)'S  0.0, 0.010000 = C(40) TO C(41) 
U(IJ)'S  0.0, 0.010000 = C(39) TO C(40) 
U(IJ)'S  0.0, 0.010000 = C(35) TO C(36) 
U(IJ)'S  0.0, 0.010000 = C(36) TO C(37) 
U(IJ)'S  0.0, 0.010000 = C(37) TO C(38) 
END                                                                             
;