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_7054953
_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         'C19 H33 Br Ni O2 P2'
_chemical_formula_sum            'C19 H33 Br Ni O2 P2'
_chemical_formula_weight         494.01
_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                102.3140(10)
_cell_angle_beta                 94.6990(10)
_cell_angle_gamma                91.9580(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3325(2)
_cell_length_b                   10.9016(2)
_cell_length_c                   12.7875(3)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.15
_cell_measurement_theta_min      4.16
_cell_volume                     1129.46(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 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11375
_diffrn_reflns_theta_full        67.42
_diffrn_reflns_theta_max         67.42
_diffrn_reflns_theta_min         4.16
_exptl_absorpt_coefficient_mu    4.720
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+0.0593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                3598
_reflns_number_total             3892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00807g2.cif
_cod_data_source_block           ds
_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_cell_volume        1129.45(4)
_cod_original_sg_symbol_Hall     ' -P 1'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054953