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_7055638
_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_absolute_configuration ad
_chemical_formula_moiety         'C35 H51 Br N3 Ni O4, C2 H6 O, Br'
_chemical_formula_sum            'C37 H57 Br2 N3 Ni O5'
_chemical_formula_weight         842.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-06-09 deposited with the CCDC.
2016-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.859(3)
_cell_length_b                   16.766(4)
_cell_length_c                   16.883(4)
_cell_measurement_reflns_used    12782
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4771
_cell_measurement_theta_min      2.1931
_cell_volume                     4206.0(16)
_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, 2014)'
_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 0.985
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.0875
              2theta: -19.9968
;
_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      0.0149
_diffrn_orient_matrix_UB_12      0.0586
_diffrn_orient_matrix_UB_13      -0.0295
_diffrn_orient_matrix_UB_21      0.0409
_diffrn_orient_matrix_UB_22      0.0108
_diffrn_orient_matrix_UB_23      0.0421
_diffrn_orient_matrix_UB_31      0.0411
_diffrn_orient_matrix_UB_32      -0.0270
_diffrn_orient_matrix_UB_33      -0.0330
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16609
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.701
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7820
_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    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 2951 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         9342
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0252P)^2^+1.6205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                8503
_reflns_number_total             9342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00559d2.cif
_cod_data_source_block           sa4499
_cod_depositor_comments
'Adding full bibliography for 7055637--7055638.cif.'
_cod_original_cell_volume        4205.9(16)
_cod_database_code               7055638
_diffrn_number_total             5284
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(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
 O4-H4
 0.85 with sigma of 0.01
 C32-H3
 1.902824 with sigma of 0.02
 Ni1-H3
 2.775309 with sigma of 0.02
 C34-H4
 1.902533 with sigma of 0.02
 Ni1-H4
 2.565939 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C36A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H5B)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C36A)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=1-FVAR(1)
 Sof(H5A)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C26(H26), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C34(H34A,H34B), C37(H37A,H37B), C37A(H37C,H37D)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3A), C3(H3B), C4(H4A), C5(H5), C10(H10), C11(H11), C12(H12),
 C22(H22), C23(H23), C24(H24)
5.d Tetrahedral OH refined with riding coordinates:
 O5(H5A), O5(H5B)
5.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              54085
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'