Simplified and versatile access to low valent Ni complexes by metal-free reduction of Ni<sup>II</sup> precursors.
Moser, Emile; Jeanneau, Erwann; Mézailles, Nicolas; Olivier-Bourbigou, Hélène; Breuil, Pierre-Alain R; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4101–4104; doi:10.1039/c9dt00668k

data_7049107
_publ_section_title
;
 Simplified and versatile access to low valent Ni complexes by metal-free
 reduction of Ni<sup>II</sup> precursors.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4101
_journal_page_last               4104
_journal_paper_doi               10.1039/c9dt00668k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C18 H41 Ni1 O1 P1 Si2'
_chemical_formula_sum            'C18 H41 Ni O P Si2'
_chemical_formula_weight         419.38
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2019-01-14 deposited with the CCDC.    2019-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                64.563(9)
_cell_angle_beta                 81.647(7)
_cell_angle_gamma                80.817(7)
_cell_formula_units_Z            2
_cell_length_a                   9.745(8)
_cell_length_b                   11.1357(11)
_cell_length_c                   11.7289(11)
_cell_measurement_reflns_used    8798
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.0020
_cell_measurement_theta_min      2.9600
_cell_volume                     1130.5(9)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_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_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29745
_diffrn_reflns_theta_full        26.151
_diffrn_reflns_theta_max         29.283
_diffrn_reflns_theta_min         3.100
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.89
_refine_diff_density_min         -1.00
_refine_ls_extinction_coef       27(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         5685
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.0006315
_refine_ls_shift/su_mean         0.0000372
_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: 
 0.173E+04 0.171E+04 958. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0752
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0752
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -13
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4505
_reflns_number_total             5695
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.44
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_r_factor_ref   0.0631
_oxford_refine_ls_scale          8.07(18)
_oxford_reflns_number_all        5685
_cod_data_source_file            c9dt00668k2.cif
_cod_data_source_block           I_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7049106--7049107.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C18 H41 Ni1 O1 P1 Si2'
_cod_database_code               7049107
_oxdiff_exptl_absorpt_empirical_full_min 0.752
_oxdiff_exptl_absorpt_empirical_full_max 1.299
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)