Synthesis and characterization of tetrapodal nickel complexes with adaptable ligand binding geometries.
Cho, Hsien-Liang; Gullett, Kelly L.; Fout, Alison R.; Chemical communications (Cambridge, England) 60 (2024) 10564–10567; doi:10.1039/d4cc03186e

data_7133683
_publ_section_title
;
 Synthesis and characterization of tetrapodal nickel complexes with
 adaptable ligand binding geometries.
;
_journal_issue                   76
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10564
_journal_page_last               10567
_journal_paper_doi               10.1039/d4cc03186e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '2(C41 H45 N7 Ni), 2(C H2 Cl2)'
_chemical_formula_sum            'C84 H94 Cl4 N14 Ni2'
_chemical_formula_weight         1558.95
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0610(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.7270(2)
_cell_length_b                   8.71219(5)
_cell_length_c                   22.27255(11)
_cell_measurement_reflns_used    78644
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.5020
_cell_measurement_theta_min      3.4230
_cell_volume                     7495.82(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.103a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.103a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.103a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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   -118.00 -69.00   0.50    2.20    --  -47.72-132.00 138.00   98
  2  \w    -91.00 -17.00   0.50    2.20    --  -47.72 132.00-151.00  148
  3  \w   -119.00 -65.00   0.50    2.20    --  -47.72-138.00 -37.00  108
  4  \w    -96.00 -20.00   0.50    2.20    --  -47.72 138.00  23.00  152
  5  \w     42.00 103.00   0.50    2.20    --   47.72-138.00 -37.00  122
  6  \w     38.00  98.00   0.50    2.20    --   47.72-132.00 138.00  120
  7  \w   -158.00 -65.00   0.50   10.00    --  -91.75-138.00 -37.00  186
  8  \w     43.00 117.00   0.50   10.00    --  113.25-132.00 138.00  148
  9  \w     42.00 121.00   0.50   10.00    --  113.25-138.00 -37.00  158
 10  \w     91.00 178.00   0.50   10.00    --  113.25 132.00-151.00  174
 11  \w     87.00 175.00   0.50   10.00    --  113.25 138.00  23.00  176
 12  \w     42.00 121.00   0.50   10.00    --  113.25-138.00 -37.00  158
 13  \w    -13.00  28.00   0.50    2.20    --  -47.72  19.00  60.00   82
 14  \w    -13.00  28.00   0.50    2.20    --  -47.72  19.00 150.00   82
 15  \w    -13.00  28.00   0.50    2.20    --  -47.72  19.00-180.00   82
 16  \w    -27.00  12.00   0.50    2.20    --   47.72 -19.00 120.00   78
 17  \w    -27.00  12.00   0.50    2.20    --   47.72 -19.00-120.00   78
 18  \w    -49.00 -20.00   0.50   10.00    --  -91.75  45.00  90.00   58
 19  \w    -91.00 -21.00   0.50   10.00    --  -91.75 132.00-151.00  140
 20  \w    -49.00 -20.00   0.50   10.00    --  -91.75  45.00  60.00   58
 21  \w     42.00  75.00   0.50   10.00    --  113.25 -61.00-180.00   66
 22  \w    110.00 178.00   0.50   10.00    --  113.25  77.00  90.00  136
 23  \w    101.00 178.00   0.50   10.00    --  113.25  45.00 -60.00  154
 24  \w    106.00 178.00   0.50   10.00    --  113.25  61.00 150.00  144
 25  \w     42.00 106.00   0.50   10.00    --  113.25 -95.00 -30.00  128
 26  \w     42.00 106.00   0.50   10.00    --  113.25 -95.00 150.00  128
 27  \w    106.00 178.00   0.50   10.00    --  113.25  61.00 120.00  144
 28  \w     42.00 136.00   0.50   10.00    --  113.25 -77.00 -30.00  188
 29  \w    101.00 178.00   0.50   10.00    --  113.25  45.00   0.00  154
 30  \w     42.00  75.00   0.50   10.00    --  113.25 -61.00 120.00   66
 31  \w    106.00 178.00   0.50   10.00    --  113.25  61.00 -90.00  144
 32  \w    106.00 178.00   0.50   10.00    --  113.25  61.00 150.00  144
 33  \w     42.00  75.00   0.50   10.00    --  113.25 -61.00 150.00   66
 34  \w   -121.00 -35.00   0.50    2.20    --  -47.72 -38.00-120.00  172
 35  \w     36.00 121.00   0.50    2.20    --   47.72  38.00 120.00  170
 36  \w     36.00 121.00   0.50    2.20    --   47.72  38.00  60.00  170
 37  \w     36.00 121.00   0.50    2.20    --   47.72  38.00-120.00  170
 38  \w     36.00 121.00   0.50    2.20    --   47.72  38.00   0.00  170
 39  \w     36.00 121.00   0.50    2.20    --   47.72  38.00-150.00  170
 40  \w     36.00 121.00   0.50    2.20    --   47.72  38.00 150.00  170
 41  \w   -163.00 -79.00   0.50   10.00    --  -91.75 -45.00  60.00  168
 42  \w    101.00 171.00   0.50   10.00    --  113.25  30.00-150.00  140
;
_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      -0.0023366000
_diffrn_orient_matrix_UB_12      -0.1756240000
_diffrn_orient_matrix_UB_13      -0.0071987000
_diffrn_orient_matrix_UB_21      -0.0116058000
_diffrn_orient_matrix_UB_22      0.0199872000
_diffrn_orient_matrix_UB_23      -0.0671509000
_diffrn_orient_matrix_UB_31      0.0380768000
_diffrn_orient_matrix_UB_32      -0.0047568000
_diffrn_orient_matrix_UB_33      -0.0157772000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            141776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.441
_diffrn_reflns_theta_min         2.287
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.103a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.450
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         15972
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0796P)^2^+15.0104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14796
_reflns_number_total             15972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03186e2.cif
_cod_data_source_block           exp_159_auto
_cod_depositor_comments
'Adding full bibliography for 7133679--7133683.cif.'
_cod_original_cell_volume        7495.83(7)
_cod_database_code               7133683
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNNiCl
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C83-Cl4 \\sim C83-Cl4A
 with sigma of 0.02
3. Others
 Sof(H83C)=Sof(H83D)=Sof(Cl4A)=1-FVAR(1)
 Sof(H83A)=Sof(H83B)=Sof(Cl4)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C36(H36), C25(H25), C77(H77), C66(H66)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C26(H26A,H26B), C29(H29A,H29B), C39(H39A,H39B), C27(H27A,
 H27B), C40(H40A,H40B), C28(H28A,H28B), C37(H37A,H37B), C41(H41A,H41B),
 C38(H38A,H38B), C67(H67A,H67B), C81(H81A,H81B), C68(H68A,H68B), C80(H80A,H80B),
  C70(H70A,H70B), C78(H78A,H78B), C79(H79A,H79B), C69(H69A,H69B), C71(H71A,
 H71B), C82(H82A,H82B), C83(H83A,H83B), C83(H83C,H83D), C84(H84A,H84B)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C35(H35), C22(H22), C24(H24), C21(H21), C9(H9), C4(H4), C10(H10),
 C3(H3), C32(H32), C33(H33), C16(H16), C15(H15), C1(H1), C11(H11), C12(H12),
 C2(H2), C62(H62), C57(H57), C55(H55), C76(H76), C74(H74), C65(H65), C50(H50),
 C44(H44), C73(H73), C43(H43), C42(H42), C51(H51), C52(H52), C53(H53), C63(H63),
  C45(H45), C56(H56)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C7(H7A,H7B,H7C), C60(H60A,H60B,H60C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              78570
_shelx_hkl_checksum              73431
_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 1.352
_oxdiff_exptl_absorpt_empirical_full_min 0.623