N<sub>3</sub>-Ligated nickel(ii) diketonate complexes: synthesis, characterization and evaluation of O<sub>2</sub> reactivity.
Elsberg, Josiah G. D.; Peterson, Austin; Fuller, Amy L.; Berreau, Lisa M.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7564–7575; doi:10.1039/d0dt01338b

data_7704437
_publ_section_title
;
 N<sub>3</sub>-Ligated nickel(ii) diketonate complexes: synthesis,
 characterization and evaluation of O<sub>2</sub> reactivity.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7564
_journal_page_last               7575
_journal_paper_doi               10.1039/d0dt01338b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C26 H32 N3 Ni O3, Cl O4'
_chemical_formula_sum            'C26 H32 Cl N3 Ni O7'
_chemical_formula_weight         592.70
_chemical_name_systematic        '[(TERPY)NiTbutyl-diketonate]ClO4'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-03-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-24 deposited with the CCDC.	2020-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                110.337(3)
_cell_angle_beta                 91.439(2)
_cell_angle_gamma                113.304(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9556(2)
_cell_length_b                   11.6346(4)
_cell_length_c                   14.2457(4)
_cell_measurement_reflns_used    10275
_cell_measurement_temperature    102(3)
_cell_measurement_theta_max      30.3610
_cell_measurement_theta_min      2.0780
_cell_volume                     1395.43(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.940
_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    -72.00 -23.00   0.50    3.45    --   20.00  54.00  30.00   98
  2  \w      0.00  38.00   0.50    3.45    --   20.00  54.00 150.00   76
  3  \w    -71.00  69.00   0.50    3.45    --   20.00  54.00 -30.00  280
  4  \w     75.00 110.00   0.50    3.45    --   20.00  54.00 -30.00   70
  5  \w    -72.00 -46.00   0.50    3.45    --   20.00  54.00-150.00   52
  6  \w    -28.00 110.00   0.50    3.45    --   20.00  54.00-150.00  276
  7  \w    -68.00 -40.00   0.50    3.45    --   20.00  54.00   0.00   56
  8  \w     -4.00  31.00   0.50    3.45    --   20.00  54.00   0.00   70
  9  \w     58.00  99.00   0.50    3.45    --   20.00  54.00   0.00   82
 10  \w    -72.00 -43.00   0.50    3.45    --   20.00  54.00-120.00   58
 11  \w      5.00 100.00   0.50    3.45    --   20.00  54.00-120.00  190
 12  \w    -74.00 -46.00   0.50    3.45    --   20.00  54.00 120.00   56
 13  \w     -1.00  24.00   0.50    3.45    --   20.00  54.00 120.00   50
 14  \w     35.00  60.00   0.50    3.45    --   20.00  54.00 120.00   50
 15  \w     85.00 110.00   0.50    3.45    --   20.00  54.00 120.00   50
 16  \w    -26.00  -1.00   0.50    3.45    --   20.00  54.00  60.00   50
 17  \w    -63.00 -36.00   0.50    3.45    --   20.00  54.00  54.96   54
 18  \w     -5.00  20.00   0.50    3.45    --   20.00  54.00  54.96   50
 19  \w     52.00  78.00   0.50    3.45    --   20.00  54.00  54.96   52
 20  \w    -64.00  82.00   0.50    3.45    --   20.00  54.00 -90.00  292
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0115902000
_diffrn_orient_matrix_UB_12      0.0577074000
_diffrn_orient_matrix_UB_13      -0.0111528000
_diffrn_orient_matrix_UB_21      -0.0385521000
_diffrn_orient_matrix_UB_22      0.0205665000
_diffrn_orient_matrix_UB_23      0.0389200000
_diffrn_orient_matrix_UB_31      0.0679687000
_diffrn_orient_matrix_UB_32      0.0379539000
_diffrn_orient_matrix_UB_33      0.0358436000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25025
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.608
_diffrn_reflns_theta_min         2.268
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       prism
_exptl_crystal_F_000             620
_exptl_crystal_preparation       'See Literature'
_exptl_crystal_recrystallization_method
'Crystallized in CH2Cl2 w one drop CH3CN and EtO2'
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.181
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         8096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0338P)^2^+0.5155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6744
_reflns_number_total             8096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01338b2.cif
_cod_data_source_block           usu_terpy_ni_tbutyl
_cod_depositor_comments
'Adding full bibliography for 7704434--7704437.cif.'
_cod_original_cell_volume        1395.42(8)
_cod_database_code               7704437
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni1 C26 H32 Cl1 O7 N3'
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C21(H21)
2.b Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C24(H24a,H24b,
 H24c), C25(H25a,H25b,H25c), C26(H26a,H26b,H26c)
;
_shelx_res_checksum              55756
_olex2_exptl_crystal_mounting_method 'Mounted on a loop with paratone oil'
_olex2_submission_original_sample_id USU_TERPY_Ni_Tbutyl
_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 1.093
_oxdiff_exptl_absorpt_empirical_full_min 0.940