Nickel(ii) complexes of a 3N ligand as a model for diketone cleaving unusual nickel(ii)-dioxygenase enzymes.
Ramasubramanian, Ramamoorthy; Anandababu, Karunanithi; Kumar, Mukesh; Mayilmurugan, Ramasamy; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4049–4053; doi:10.1039/c7dt04739h

data_7045620
_publ_section_title
;
 Nickel(ii) complexes of a 3N ligand as a model for diketone cleaving
 unusual nickel(ii)-dioxygenase enzymes.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4049
_journal_page_last               4053
_journal_paper_doi               10.1039/c7dt04739h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C34 H39 N6 Ni O2, Cl O4'
_chemical_formula_sum            'C34 H39 Cl N6 Ni O6'
_chemical_formula_weight         721.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-08-17 deposited with the CCDC.
2018-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                76.449(3)
_cell_angle_beta                 88.375(3)
_cell_angle_gamma                76.193(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5304(4)
_cell_length_b                   10.1589(4)
_cell_length_c                   19.4742(7)
_cell_measurement_reflns_used    7117
_cell_measurement_temperature    293
_cell_measurement_theta_max      73.0400
_cell_measurement_theta_min      4.5980
_cell_volume                     1779.25(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1600
_diffrn_detector_type            Titan
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.957
_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      5.00  92.00   1.00    1.00    --   43.29-126.00-150.00   87
  2  \w     69.00  95.00   1.00    1.00    --   43.29-126.00 -30.00   26
  3  \w    109.00 134.00   1.00    1.18    --  102.90 -77.00 -30.00   25
  4  \w     86.00 122.00   1.00    1.18    --  102.90-126.00-150.00   36
  5  \w     58.00  89.00   1.00    1.18    --  102.90 -95.00-120.00   31
  6  \w     31.00  99.00   1.00    1.18    --  102.90 -95.00 -60.00   68
  7  \w     32.00  64.00   1.00    1.18    --  102.90 -77.00 -30.00   32
  8  \w     30.00 104.00   1.00    1.18    --  102.90 -95.00  30.00   74
  9  \w     59.00 109.00   1.00    1.18    --  102.90 -95.00 120.00   50
 10  \w     45.00 128.00   1.00    1.18    --  102.90 -45.00 120.00   83
 11  \w     64.00 152.00   1.00    1.18    --  102.90  15.00  30.00   88
 12  \w     81.00 155.00   1.00    1.18    --  102.90  77.00  90.00   74
 13  \w     76.00 158.00   1.00    1.18    --  102.90  61.00  60.00   82
 14  \w    103.00 149.00   1.00    1.18    --  102.90 126.00 -90.00   46
 15  \w    127.00 156.00   1.00    1.18    --  102.90  45.00-150.00   29
 16  \w     90.00 117.00   1.00    1.18    --  102.90  45.00-150.00   27
 17  \w   -108.00 -21.00   1.00    1.00    --  -43.29 -38.00 -90.00   87
 18  \w   -121.00 -11.00   1.00    1.00    --  -43.29 -19.00   0.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0779798000
_diffrn_orient_matrix_UB_12      0.0421646000
_diffrn_orient_matrix_UB_13      -0.0728842000
_diffrn_orient_matrix_UB_21      -0.0569840000
_diffrn_orient_matrix_UB_22      -0.1334259000
_diffrn_orient_matrix_UB_23      0.0184137000
_diffrn_orient_matrix_UB_31      -0.1356606000
_diffrn_orient_matrix_UB_32      0.0788864000
_diffrn_orient_matrix_UB_33      0.0312421000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12699
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.219
_diffrn_reflns_theta_min         4.611
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.905
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.569
_exptl_crystal_size_mid          0.333
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1206P)^2^+1.0998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1907
_refine_ls_wR_factor_ref         0.2156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5153
_reflns_number_total             6839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04739h2.cif
_cod_data_source_block           rnbia_1
_cod_depositor_comments
'Adding full bibliography for 7045620--7045621.cif.'
_cod_original_cell_volume        1779.24(13)
_cod_database_code               7045620
_chemical_oxdiff_formula         'C34 H39 Cl N6 Ni O6'
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C17(H17),
 C18(H18), C19(H19), C20(H20), C29(H29)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-04-03
_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 1.765
_oxdiff_exptl_absorpt_empirical_full_min 0.607