Synthesis of unsymmetrical 5,6-POCOP′-type pincer complexes of nickel(ii): impact of nickelacycle size on structures and spectroscopic properties
Salah, Abderrahmen; Corpet, Martin; ul-Hassan Khan, Najm; Zargarian, Davit; Spasyuk, Denis M.; New J. Chem. 39 (2015) 6649–; doi:10.1039/C5NJ00807G

data_7054957
_publ_section_title
;
 Synthesis of unsymmetrical 5,6-POCOP&#x2032;-type pincer complexes of
 nickel(ii): impact of nickelacycle size on structures and spectroscopic
 properties
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              6649
_journal_paper_doi               10.1039/C5NJ00807G
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C20 H36 Ni O2 P2 '
_chemical_formula_sum            'C20 H36 Ni O2 P2'
_chemical_formula_weight         429.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-05 deposited with the CCDC.
2015-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                102.6810(10)
_cell_angle_beta                 94.2040(10)
_cell_angle_gamma                92.4430(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3833(2)
_cell_length_b                   10.8596(2)
_cell_length_c                   12.7379(3)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.99
_cell_measurement_theta_min      3.57
_cell_volume                     1126.26(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Platon Ortep'
_computing_publication_material  'LinXTL v.  3.8.1'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18147
_diffrn_reflns_theta_full        67.96
_diffrn_reflns_theta_max         67.96
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    2.655
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.6298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                3918
_reflns_number_total             4006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00807g2.cif
_cod_data_source_block           dens53
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7054953--7054957.cif.
;
_cod_original_sg_symbol_Hall     ' -P 1'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054957