Bidentate forms of β-triketimines: syntheses, characterization and outstanding performance of enamine-diimine cobalt complexes in isoprene polymerization.
Alnajrani, Mohammed N.; Mair, Francis S.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10435–10446; doi:10.1039/c6dt01064d

data_7040201
_publ_section_title
;
 Bidentate forms of \b-triketimines: syntheses, characterization and
 outstanding performance of enamine-diimine cobalt complexes in isoprene
 polymerization.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10435
_journal_page_last               10446
_journal_paper_doi               10.1039/c6dt01064d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C34 H43 Br2 Co N3, 1.01(C5.95 H3.97 Cl2)'
_chemical_formula_sum            'C40 H47 Br2 Cl2 Co N3'
_chemical_formula_weight         859.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.021(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6906(11)
_cell_length_b                   14.9680(10)
_cell_length_c                   17.0951(13)
_cell_measurement_reflns_used    5044
_cell_measurement_temperature    150.01(13)
_cell_measurement_theta_max      27.5540
_cell_measurement_theta_min      3.8340
_cell_volume                     3992.8(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details
;
  1 omega  -51.00  -17.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9725   57.0000    0.0000 34

  2 omega  -98.00   17.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9725   19.0000  150.0000 115

  3 omega  -15.00   21.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9725  -99.0000   30.0000 36

  4 omega   42.00   86.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0662  178.0000  -30.0000 44

  5 omega  -23.00    2.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9725  -96.0000 -142.0000 25

  6 omega    1.00   26.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9725  -99.0000 -150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0159058000
_diffrn_orient_matrix_UB_12      0.0442994000
_diffrn_orient_matrix_UB_13      0.0015708000
_diffrn_orient_matrix_UB_21      0.0099572000
_diffrn_orient_matrix_UB_22      0.0075062000
_diffrn_orient_matrix_UB_23      -0.0389941000
_diffrn_orient_matrix_UB_31      -0.0414163000
_diffrn_orient_matrix_UB_32      -0.0150777000
_diffrn_orient_matrix_UB_33      -0.0146802000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17840
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.714
_diffrn_reflns_theta_min         3.281
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_F_000             1756
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.890
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         8966
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0524P)^2^+0.9430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5405
_reflns_number_total             8966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01064d2.cif
_cod_data_source_block           II
_cod_database_code               7040201
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C34H43N3Co1Br2
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C40B, C1A}
{C1B, C36B}
{Cl38, C1H}
{Cl1, C2A}
3. Restrained distances
 C39A-Cl1 \\sim Cl1-C37A
 with sigma of 0.02
 C37B-C36B \\sim C36B-C35B
 with sigma of 0.02
 C35A-C40B \\sim C40B-C39A
 with sigma of 0.02
 C35A-C36B \\sim C36B-C37A
 with sigma of 0.02
 C35B-C40B \\sim C40B-C39B
 with sigma of 0.02
 C37B-Cl38 \\sim Cl38-C39B
 with sigma of 0.02
4. Rigid bond restraints
 Cl2A, Cl2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2A, Cl2B, C36B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Cl2B \\sim Cl2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(Cl1) = Uanis(C2A)
Uanis(Cl1) = Uanis(C2A)
Uanis(C1A) = Uanis(C40B)
Uanis(C40B) = Uanis(C1A)
Uanis(C36B) = Uanis(C1B)
Uanis(C1B) = Uanis(C36B)
Uanis(C1H) = Uanis(Cl38)
Uanis(Cl38) = Uanis(C1H)
6. Rigid body (RIGU) restrains
 C39B, Cl1, C35B, C1A, C36B, Cl2B, C37B, C1H, Cl2A, Cl38, C35A, C1B, C40B,
 C37A, C39A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(Cl1)=Sof(Cl2B)=Sof(C1A)=Sof(H1AA)=Sof(C36B)=Sof(C1H)=Sof(H1H)=1-FVAR(1)
 Sof(Cl38)=Sof(C1B)=Sof(Cl2A)=Sof(C40B)=Sof(H40B)=Sof(C2A)=Sof(H2A)=FVAR(1)
 Fixed Sof: C39A(0.5) H39A(0.5) C35A(0.5) C39B(0.5) H39B(0.5) C35B(0.5)
 C37B(0.5) H37B(0.5) C37A(0.5) H37A(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C19(H19), C21(H21), C30(H30), C12(H12), C28(H28), C10(H10), C1A(H1AA),
  C39A(H39A), C39B(H39B), C37B(H37B), C40B(H40B), C1H(H1H), C2A(H2A), C37A(H37A)
8.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C1(H1A,H1B,H1C), C33(H33A,H33B,H33C), C5(H5A,H5B,H5C),
 C7(H7A,H7B,H7C), C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C25(H25A,H25B,H25C),
  C23(H23A,H23B,H23C), C34(H34A,H34B,H34C), C14(H14A,H14B,H14C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              17428
_olex2_submission_special_instructions 'No special instructions were received'