Ni(2,2':6',2''-terpyridine)<sub>2</sub>: a high-spin octahedral formal Ni(0) complex.
Cabrera-Lobera, Natalia; Del Horno, Estefanía; Quirós, M Teresa; Buñuel, Elena; Gimeno, Magali; Brennessel, William W.; Neidig, Michael L.; Priego, José Luis; Cárdenas, Diego J; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8550–8554; doi:10.1039/d3dt04247b

data_7715902
_publ_section_title
;
 Ni(2,2':6',2''-terpyridine)<sub>2</sub>: a high-spin octahedral formal
 Ni(0) complex.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8550
_journal_page_last               8554
_journal_paper_doi               10.1039/d3dt04247b
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H22 N6 Ni'
_chemical_formula_sum            'C30 H22 N6 Ni'
_chemical_formula_weight         525.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-12-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-14 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   56.2329(5)
_cell_length_b                   39.4759(4)
_cell_length_c                   8.49770(10)
_cell_measurement_reflns_used    23899
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      77.1270
_cell_measurement_theta_min      3.1640
_cell_volume                     18863.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -40.00  12.00   0.50    7.09    --  -49.62  19.00 -60.00  104
  2  \w    -36.00 -11.00   0.50   28.37    --  -84.25  19.00 -30.00   50
  3  \w    -52.00  21.00   0.50    7.09    --  -49.62  19.00-120.00  146
  4  \w     55.00  80.00   0.50    7.09    --   49.62-126.00  10.00   50
  5  \w     32.00  57.00   0.50   28.37    --  105.75 -19.00 -30.00   50
  6  \w     54.00 109.00   0.50   28.37    --  105.75 -99.00-150.00  110
  7  \w     55.00  80.00   0.50   28.37    --  105.75 -38.00-150.00   50
  8  \w     36.00  74.00   0.50   28.37    --  105.75 -38.00-180.00   76
  9  \w     42.00 125.00   0.50   28.37    --  105.75-144.00-157.00  166
 10  \w     34.00  70.00   0.50   28.37    --  105.75 -19.00 120.00   72
 11  \w    111.00 136.00   0.50   28.37    --  105.75 126.00  87.00   50
 12  \w    -99.00 -57.00   0.50   28.37    --  -84.25-144.00-157.00   84
 13  \w   -113.00 -88.00   0.50    7.09    --  -49.62-144.00-157.00   50
 14  \w   -156.00-123.00   0.50   28.37    --  -84.25-126.00  10.00   66
 15  \w   -114.00 -81.00   0.50    7.09    --  -49.87-125.00-120.00   66
 16  \w    -34.00  -8.00   0.50    7.09    --  -49.87  19.00  90.00   52
 17  \w     37.00  69.00   0.50   28.37    --  105.75 -19.00-180.00   64
 18  \w     87.00 113.00   0.50   28.37    --  105.75-125.00 -30.00   52
 19  \w     36.00  75.00   0.50   28.37    --  105.75-125.00 -30.00   78
 20  \w     35.00  61.00   0.50   28.37    --  105.75 -19.00  90.00   52
 21  \w     79.00 116.00   0.50   28.37    --  105.75 -57.00   0.00   74
 22  \w     38.00  64.00   0.50   28.37    --  105.75 -99.00   0.00   52
 23  \w     79.00 105.00   0.50   28.37    --  105.75 -99.00   0.00   52
 24  \w     41.00  67.00   0.50   28.37    --  105.75 -19.00-120.00   52
 25  \w     35.00  65.00   0.50   28.37    --  105.75 -57.00   0.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0179556000
_diffrn_orient_matrix_UB_12      0.0294546000
_diffrn_orient_matrix_UB_13      -0.0036101000
_diffrn_orient_matrix_UB_21      0.0206312000
_diffrn_orient_matrix_UB_22      -0.0255780000
_diffrn_orient_matrix_UB_23      -0.0107861000
_diffrn_orient_matrix_UB_31      -0.0015720000
_diffrn_orient_matrix_UB_32      0.0009493000
_diffrn_orient_matrix_UB_33      -0.1809552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            31051
_diffrn_reflns_point_group_measured_fraction_full 0.704
_diffrn_reflns_point_group_measured_fraction_max 0.667
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.880
_diffrn_reflns_theta_min         2.735
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       needle
_exptl_crystal_F_000             8704
_exptl_crystal_size_max          0.589
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         6724
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+14.0834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.275
_reflns_Friedel_fraction_full    0.362
_reflns_Friedel_fraction_max     0.309
_reflns_number_gt                6557
_reflns_number_total             6724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04247b2.cif
_cod_data_source_block           neinc08
_cod_depositor_comments          'Adding full bibliography for 7715902.cif.'
_cod_database_code               7715902
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.484
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.56(3)
 0.44(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53),
 C54(H54), C57(H57), C58(H58), C59(H59), C60(H60)
;
_shelx_res_checksum              41832
_olex2_submission_original_sample_id neinc08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.835
_oxdiff_exptl_absorpt_empirical_full_min 0.427