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_7045621
_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         'C36 H30 N5 Ni O3, Cl'
_chemical_formula_sum            'C36 H30 Cl N5 Ni O3'
_chemical_formula_weight         674.81
_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
_audit_creation_date             2017-05-16
_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                90
_cell_angle_beta                 98.049(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1764(4)
_cell_length_b                   13.0535(6)
_cell_length_c                   26.4288(9)
_cell_measurement_reflns_used    6094
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.8950
_cell_measurement_theta_min      3.7740
_cell_volume                     3134.6(2)
_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 0.987
_diffrn_measured_fraction_theta_max 0.960
_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    -67.00  23.00   1.00   10.00    --  -43.54  38.00 -60.00   90
  2  \w   -125.00 -81.00   1.00   10.00    --  -43.54 -99.00-180.00   44
  3  \w   -125.00 -80.00   1.00   10.00    --  -43.54 -99.00 -90.00   45
  4  \w     35.00 130.00   1.00   60.00    --  102.90 -61.00-150.00   95
  5  \w     86.00 112.00   1.00   60.00    --  102.90  45.00-150.00   26
  6  \w    132.00 157.00   1.00   60.00    --  102.90  45.00-150.00   25
  7  \w     71.00 155.00   1.00   60.00    --  102.90  77.00   0.00   84
  8  \w    127.00 153.00   1.00   60.00    --  102.90   0.00  30.00   26
  9  \w     73.00  99.00   1.00   60.00    --  102.90   0.00  30.00   26
 10  \w     38.00  91.00   1.00   60.00    --  102.90 -95.00 150.00   53
 11  \w     25.00  51.00   1.00   60.00    --  102.90   0.00  30.00   26
 12  \w     79.00 148.00   1.00   60.00    --  102.90 126.00-120.00   69
;
_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      0.0233028000
_diffrn_orient_matrix_UB_12      0.0073771000
_diffrn_orient_matrix_UB_13      0.0587173000
_diffrn_orient_matrix_UB_21      -0.0813367000
_diffrn_orient_matrix_UB_22      -0.1027045000
_diffrn_orient_matrix_UB_23      0.0031580000
_diffrn_orient_matrix_UB_31      0.1468199000
_diffrn_orient_matrix_UB_32      -0.0579771000
_diffrn_orient_matrix_UB_33      0.0019801000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            12384
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.194
_diffrn_reflns_theta_min         3.378
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.046
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.696
_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    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.626
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1053P)^2^+2.5098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.2238
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4628
_reflns_number_total             6043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04739h2.cif
_cod_data_source_block           rnib5_2
_cod_depositor_comments
'Adding full bibliography for 7045620--7045621.cif.'
_cod_database_code               7045621
_chemical_oxdiff_formula         'Ni C36 H30 Cl N5 O3'
_reflns_odcompleteness_completeness 99.47
_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, All O(H,H) groups
2.a Rotating group:
 O3(H3A,H3B)
2.b 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), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C29(H29), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-05-15
_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 2.675
_oxdiff_exptl_absorpt_empirical_full_min 0.380