Synthesis and characterization of β-triketimine cobalt complexes and their behaviour in the polymerization of 1,3-butadiene.
Alnajrani, Mohammed N.; Mair, Francis S.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15727–15736; doi:10.1039/c4dt02196g

data_7032236
_publ_section_title
;
 Synthesis and characterization of \b-triketimine cobalt complexes and
 their behaviour in the polymerization of 1,3-butadiene.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15727
_journal_page_last               15736
_journal_paper_doi               10.1039/c4dt02196g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C62 H74 Br2 Co2 N6 O2, C H2 Cl2, 2(C32 H12 B F24)'
_chemical_formula_sum            'C127 H100 B2 Br2 Cl2 Co2 F48 N6 O2'
_chemical_formula_weight         3024.33
_chemical_melting_point          490
_chemical_name_common            'L3CoBr BArF dimer'
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                81.320(4)
_cell_angle_beta                 73.034(5)
_cell_angle_gamma                83.347(4)
_cell_formula_units_Z            1
_cell_length_a                   13.4133(7)
_cell_length_b                   15.7628(8)
_cell_length_c                   16.2244(9)
_cell_measurement_reflns_used    13798
_cell_measurement_temperature    150
_cell_measurement_theta_max      74.6560
_cell_measurement_theta_min      2.8390
_cell_volume                     3234.1(3)
_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
;
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_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
  1 omega   43.86  221.86   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.8672  -25.7902 89

  2 omega  -86.24   37.76   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -79.5000   73.8672   91.7100 62

  3 phi    -21.86  228.10   1.9997   13.0000
omega____ theta____ kappa____ phi______ frames
 170.4096  110.0000   73.8672     -     125

  4 phi    -23.41  198.57   1.9998   13.0000
omega____ theta____ kappa____ phi______ frames
 130.5397  110.0000   73.8672     -     111

  5 phi    -25.79  174.18   1.9997   13.0000
omega____ theta____ kappa____ phi______ frames
-135.7903  110.0000   73.8672     -     100

  6 omega   85.00  227.00   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   73.8672  -30.7908 71

  7 phi    -23.29  192.71   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
 119.2097  111.0000   73.8672     -     108

  8 omega   82.58  198.58   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8672  -80.7912 58

  9 omega  -19.25  134.75   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000   73.8672  -55.7909 77

 10 omega  113.21  231.21   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8672 -125.7912 59

 11 omega   95.15  219.15   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8672  -45.7903 62

 12 omega  -77.63   14.37   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.0000   73.8672  134.2097 46

 13 omega    1.58   75.58   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -75.0000   73.8672   19.2097 37

 14 phi     97.90  193.89   1.9998   13.0000
omega____ theta____ kappa____ phi______ frames
-175.7903  113.0000   73.8672     -     48

 15 omega   66.19  138.19   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       -5.0000   73.8672   34.2091 36

 16 omega   82.00  152.00   2.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.8672  -88.2900 35
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.0404348000
_diffrn_orient_matrix_UB_12      -0.0902693000
_diffrn_orient_matrix_UB_13      0.0154796000
_diffrn_orient_matrix_UB_21      -0.0480647000
_diffrn_orient_matrix_UB_22      0.0245417000
_diffrn_orient_matrix_UB_23      -0.0765734000
_diffrn_orient_matrix_UB_31      0.1027495000
_diffrn_orient_matrix_UB_32      -0.0328706000
_diffrn_orient_matrix_UB_33      -0.0624840000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28209
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         2.84
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49726
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.367
_refine_diff_density_min         -2.692
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         11313
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1792P)^2^+17.6962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2776
_refine_ls_wR_factor_ref         0.2937
_reflns_number_gt                9258
_reflns_number_total             11313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02196g1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7032234--7032236.cif.'
_cod_database_code               7032236
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C65) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: C65(0.5) HL(0.5) HM(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C65(HL,HM)
4.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C23(H23), C14(H14), C53(H), C62(HA), C13(H13), C28(H28), C16(H16),
 C45(HB), C20(H20), C33(HC), C37(HD), C35(HE), C60(HF), C41(HG), C58(HH),
 C30(H30), C43(HI), C49(HJ), C56(H56), C51(HK), C15(H15), C22(H22), C27(H27)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C10(H10A,H10B,H10C),
 C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C31(H31A,H31B,H31C), C24(H24A,H24B,H24C)
;