Synthesis and characterization of a series of nickel(II) alkoxide precursors and their utility for Ni(0) nanoparticle production
Treadwell, LaRico J.; Boyle, Timothy J.; Phelan, W. Adam; Parkes, Marie V.; Young, David P.; Dalton Trans.  (2017) –; doi:10.1039/C6DT04083G

data_7042208
_publ_section_title
;
 Synthesis and characterization of a series of nickel(II) alkoxide
 precursors and their utility for Ni(0) nanoparticle production
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C6DT04083G
_journal_year                    2017
_chemical_formula_sum            'C46 H36 N2 Ni O2'
_chemical_formula_weight         707.48
_chemical_name_common            NiDPhP
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2016-10-19 deposited with the CCDC.
2017-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.902(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6216(6)
_cell_length_b                   15.5037(10)
_cell_length_c                   19.9185(12)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    102.(2)
_cell_measurement_theta_max      25.3316
_cell_measurement_theta_min      2.3820
_cell_volume                     3584.3(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      102.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53784
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.99
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.481
_refine_ls_abs_structure_details
;
Flack x determined using 5580 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         13038
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+3.4064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                12380
_reflns_number_total             13038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04083g2.cif
_cod_data_source_block           I
_cod_database_code               7042208
_shelx_res_checksum              59646