Synthesis, characterization, and crystal structures of organonickel(II) complexes coordinated to novel 1-bromo-2,6-bis{[(λ^5^-phosphanylidene)imino]methyl}benzene NCN-pincer ligands
Guillet, Gary L.; Pitts, Skyler L.; Sheriff, Kirkland W.; Rucker, Donna N.; Rogers, Aaryn L.; Acta Crystallographica Section C 75 (2019) 1381–1388; doi:10.1107/S2053229619012038

data_2021765
_publ_section_title
;
 Synthesis, characterization, and crystal structures of organonickel(II)
 complexes coordinated to novel
 1-bromo-2,6-bis{[(\l^5^-phosphanylidene)imino]methyl}benzene NCN-pincer
 ligands
;
_journal_coeditor_code           JX3045
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1381
_journal_page_last               1388
_journal_paper_doi               10.1107/S2053229619012038
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ni Br (C44 H37 N2 P2)], 0.5C2 H2 Cl2'
_chemical_formula_moiety         'C44 H37 Br N2 Ni P2, C0.5 H Cl'
_chemical_formula_sum            'C44.5 H38 Br Cl N2 Ni P2'
_chemical_formula_weight         836.78
_chemical_name_systematic
;(2,6-Bis{[(triphenyl-\l^5^-phosphanylidene)imino]methyl}phenyl-\k^3^<i>N</i>,<i>C</i>^1^,<i>N</i>')bromidonickel(II)
dichlorometahne hemisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.421(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.319(13)
_cell_length_b                   11.655(5)
_cell_length_c                   23.593(10)
_cell_measurement_reflns_used    8496
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.7
_cell_volume                     7722(6)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2009)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      170
_diffrn_detector                 'Rigaku XtaLAB area detector'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mini template'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            40203
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         1.892
_diffrn_source                   'Sealed Tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.724
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Rigaku, 1998)
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    "'not measured"
_exptl_crystal_description       block
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.667
_refine_ls_extinction_coef       0.00011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0234P)^2^+15.3313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                6363
_reflns_number_total             8846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3045sup1.cif
_cod_data_source_block           x634
_cod_depositor_comments
'Adding full bibliography for 2021765--2021768.cif.'
_cod_original_formula_sum        'C44.50 H38 Br Cl N2 Ni P2'
_cod_database_code               2021765
_cod_database_fobs_code          2021765
_shelx_estimated_absorpt_t_min   0.560
_shelx_estimated_absorpt_t_max   0.747
_shelx_hkl_checksum              13041
_shelx_res_checksum              2060