Direct C-C coupling of two Ni-salphen complexes to yield dinickel-disalphen complexes with symmetric and non-symmetric substitution-patterns.
Bugenhagen, B. E. C.; Prosenc, M. H.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 7460–7468; doi:10.1039/c5dt04612b

data_7038826
_publ_section_title
;
 Direct C-C coupling of two Ni-salphen complexes to yield
 dinickel-disalphen complexes with symmetric and non-symmetric
 substitution-patterns.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7460
_journal_page_last               7468
_journal_paper_doi               10.1039/c5dt04612b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C H Cl3, C24 H21 Br N2 Ni O2'
_chemical_formula_sum            'C25 H22 Br Cl3 N2 Ni O2'
_chemical_formula_weight         627.41
_chemical_name_common            tbu-br-salph-ni
_chemical_name_systematic
N-(5-tert-Butylsalicyliden)-N'-(5-bromsalicyliden)-phenylendiaminatonickel(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2015-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-13 deposited with the CCDC.
2016-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                84.5060(10)
_cell_angle_beta                 76.2050(10)
_cell_angle_gamma                76.1030(10)
_cell_formula_units_Z            8
_cell_length_a                   13.3441(2)
_cell_length_b                   17.1747(3)
_cell_length_c                   23.5777(4)
_cell_measurement_reflns_used    9277
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.29
_cell_volume                     5089.85(15)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            105227
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.400
_diffrn_reflns_theta_min         1.780
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.673
_exptl_absorpt_correction_T_max  0.4302
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2013/2 (Bruker,2013) was used for absorption correction.
wR2(int) was 0.0713 before and 0.0509 after correction.
The Ratio of minimum to maximum transmission is 0.9131.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       block
_exptl_crystal_F_000             2528
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform'
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.142
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         22932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+2.6217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15397
_reflns_number_total             22932
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {40dc6cc2-48f2-4ac5-bd49-d120d744e783}
_cod_data_source_file            c5dt04612b2.cif
_cod_data_source_block           tbu-br-salph-ni_bb67
_cod_depositor_comments
'Adding full bibliography for 7038824--7038828.cif.'
_cod_database_code               7038826
_shelxl_version_number           2013-4
_shelx_res_checksum              4517