Nickel(ii) complexes chelated by 2,6-pyridinedicarboxamide: syntheses, characterization, and ethylene oligomerization
Zhang, Jie; Liu, Shaofeng; Li, Antai; Ye, Hongqi; Li, Zhibo; New J. Chem. 40 (2016) 7027–; doi:10.1039/C6NJ00559D

data_7055637
_publ_section_title
;
 Nickel(ii) complexes chelated by 2,6-pyridinedicarboxamide: syntheses,
 characterization, and ethylene oligomerization
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              7027
_journal_paper_doi               10.1039/C6NJ00559D
_journal_volume                  40
_journal_year                    2016
_chemical_compound_source        no
_chemical_formula_moiety         'C28 H37 Br N3 Ni O4, O, Br'
_chemical_formula_sum            'C28 H37 Br2 N3 Ni O5'
_chemical_formula_weight         714.13
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic        Ni5
_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             2015-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-04 deposited with the CCDC.
2016-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.319(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.331(3)
_cell_length_b                   15.527(4)
_cell_length_c                   14.982(4)
_cell_measurement_reflns_used    8515
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4751
_cell_measurement_theta_min      1.9993
_cell_volume                     3139.6(13)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.0993
              2theta: -20.0068
scan:
    Number of images: 298
               Slice: -107.0000 - 42.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.0993
              2theta: -20.0068
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0600
_diffrn_orient_matrix_UB_12      0.0239
_diffrn_orient_matrix_UB_13      0.0397
_diffrn_orient_matrix_UB_21      0.0179
_diffrn_orient_matrix_UB_22      -0.0372
_diffrn_orient_matrix_UB_23      0.0494
_diffrn_orient_matrix_UB_31      0.0077
_diffrn_orient_matrix_UB_32      0.0602
_diffrn_orient_matrix_UB_33      0.0425
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22233
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         1.509
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    3.203
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7137
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0806
_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^)+(0.0283P)^2^+18.1415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6357
_reflns_number_total             7137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00559d2.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'unknown' was changed to '?' - the
value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055637--7055638.cif.
;
_cod_original_cell_volume        3139.5(13)
_cod_database_code               7055637
_diffrn_number_total             7428
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C27-C26
 1.54 with sigma of 0.01
 C28-H3
 1.879898 with sigma of 0.02
 Ni1-H3
 2.712561 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C27)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(Br2A)=1-FVAR(2)
 Sof(Br2)=FVAR(2)
5.a Rotating group:
 O4(H4A,H4B)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C24(H24A,H24B), C24(H24C,H24D), C26(H26A,H26B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3A), C2(H2), C3(H3B), C4(H4), C13(H13), C14(H14), C15(H15),
 C20(H20), C21(H21), C22(H22)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F)
;
_shelx_res_checksum              91281
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'