Neutral and cationic chiral NCN pincer nickel(ii) complexes with 1,3-bis(2'-imidazolinyl)benzenes: synthesis and characterization.
Shao, Dan-Dan; Niu, Jun-Long; Hao, Xin-Qi; Gong, Jun-Fang; Song, Mao-Ping; Dalton transactions (Cambridge, England : 2003) 40 (2011) 9012–9019; doi:10.1039/c1dt10329f

data_7016366
_publ_section_title
;
 Neutral and cationic chiral NCN pincer nickel(ii) complexes with
 1,3-bis(2'-imidazolinyl)benzenes: synthesis and characterization.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9012
_journal_page_last               9019
_journal_paper_doi               10.1039/c1dt10329f
_journal_volume                  40
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'B F4, C42 H40 N5 Ni'
_chemical_formula_sum            'C42 H40 B F4 N5 Ni'
_chemical_formula_weight         760.31
_chemical_name_systematic
;
?
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-04-11
_audit_creation_method
;
Olex2 1.1
(compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.4050(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0806(2)
_cell_length_b                   12.41579(19)
_cell_length_c                   13.7889(3)
_cell_measurement_reflns_used    3367
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      61.0113
_cell_measurement_theta_min      3.2673
_cell_volume                     1859.54(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
1 omega -105.00 -19.00 0.5000 6.0000
omega____ theta____ kappa____ phi______ frames
- -35.1548 -37.0000 -90.0000 172

2 omega -97.00 -7.00 0.5000 6.0000
omega____ theta____ kappa____ phi______ frames
- -35.1548 -77.0000 30.0000 180

3 omega 69.00 158.00 0.5000 30.0000
omega____ theta____ kappa____ phi______ frames
- 89.2441 45.0000 120.0000 178

4 omega 80.00 117.00 0.5000 30.0000
omega____ theta____ kappa____ phi______ frames
- 89.2441 -77.0000 -30.0000 74

5 omega 22.00 113.00 0.5000 30.0000
omega____ theta____ kappa____ phi______ frames
- 89.2441 -77.0000 -150.0000 182

6 omega 61.00 154.00 0.5000 30.0000
omega____ theta____ kappa____ phi______ frames
- 89.2441 15.0000 -120.0000 186

7 omega 20.00 56.00 0.5000 30.0000
omega____ theta____ kappa____ phi______ frames
- 89.2441 -77.0000 -30.0000 72

8 omega 102.00 153.00 0.5000 30.0000
omega____ theta____ kappa____ phi______ frames
- 89.2441 111.0000 60.0000 102

9 omega -82.00 -36.00 0.5000 6.0000
omega____ theta____ kappa____ phi______ frames
- -35.1548 109.0000 164.0000 92

10 omega -105.00 -5.00 0.5000 6.0000
omega____ theta____ kappa____ phi______ frames
- -35.1548 -77.0000 -180.0000 200
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1125573000
_diffrn_orient_matrix_UB_12      0.0019900000
_diffrn_orient_matrix_UB_13      0.0501210000
_diffrn_orient_matrix_UB_21      -0.0831079000
_diffrn_orient_matrix_UB_22      0.0311962000
_diffrn_orient_matrix_UB_23      -0.0993214000
_diffrn_orient_matrix_UB_31      -0.0234393000
_diffrn_orient_matrix_UB_32      -0.1200379000
_diffrn_orient_matrix_UB_33      -0.0249420000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5855
_diffrn_reflns_theta_full        61.08
_diffrn_reflns_theta_max         61.08
_diffrn_reflns_theta_min         3.27
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         4030
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0931P)^2^+0.4672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                3569
_reflns_number_total             4030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10329f.txt
_cod_data_source_block           CCDC-811901
_cod_database_code               7016366
_chemical_oxdiff_formula         'C11 H10 S O2'
_reflns_odcompleteness_completeness 72.88
_reflns_odcompleteness_iscentric 0
_reflns_odcompleteness_theta     58.86