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_7049106
_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         'C22 H36 Ni P'
_chemical_formula_sum            'C22 H36 Ni P'
_chemical_formula_weight         390.21
_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
_audit_update_record
;
2018-11-20 deposited with the CCDC.    2019-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5546(10)
_cell_length_b                   17.1029(15)
_cell_length_c                   13.3750(15)
_cell_measurement_reflns_used    8714
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4080
_cell_measurement_theta_min      3.7030
_cell_volume                     2152.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_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  0.054
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26929
_diffrn_reflns_theta_full        26.692
_diffrn_reflns_theta_max         29.761
_diffrn_reflns_theta_min         2.840
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.799
_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            yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.98
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5461
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.0007090
_refine_ls_shift/su_mean         0.0000445
_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: 
 672. 998. 511. 118. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1380
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1380
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4351
_reflns_number_total             5472
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.96
_oxford_diffrn_Wilson_scale      0.12
_oxford_refine_ls_r_factor_ref   0.0769
_oxford_refine_ls_scale          2.55(2)
_oxford_reflns_number_all        5461
_cod_data_source_file            c9dt00668k2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7049106--7049107.cif.'
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7049106
_oxdiff_exptl_absorpt_empirical_full_min 0.942
_oxdiff_exptl_absorpt_empirical_full_max 1.138
_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)