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_2021768
_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 H73 N2 P2)]'
_chemical_formula_moiety         'C44 H73 Br N2 Ni P2'
_chemical_formula_sum            'C44 H73 Br N2 Ni P2'
_chemical_formula_weight         830.60
_chemical_name_systematic
(2,6-Bis{[(tricyclohexyl-\l^5^-phosphanylidene)imino]methyl}phenyl-\k^3^<i>N</i>,<i>C</i>^1^,<i>N</i>')bromidonickel(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.521(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.569(9)
_cell_length_b                   11.612(6)
_cell_length_c                   20.608(10)
_cell_measurement_reflns_used    8356
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.8
_cell_volume                     4203(4)
_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      173
_diffrn_detector                 'Rigaku XtaLAB area detector'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_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  0.1056
_diffrn_reflns_av_unetI/netI     0.0993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.555
_diffrn_reflns_theta_min         2.013
_diffrn_source                   'Sealed Tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Rigaku, 1998)
;
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    "'not measured"
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.885
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         9621
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+6.2065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                6279
_reflns_number_total             9621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3045sup1.cif
_cod_data_source_block           x821b
_cod_depositor_comments
'Adding full bibliography for 2021765--2021768.cif.'
_cod_database_code               2021768
_cod_database_fobs_code          2021768
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.793
_shelx_hkl_checksum              65674
_shelx_res_checksum              46025