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_7040200
_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         'C38 H51 Br Co N3 O, C32 H12 B F24'
_chemical_formula_sum            'C70 H63 B Br Co F24 N3 O'
_chemical_formula_weight         1567.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-11-12
_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                 114.988(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.4767(19)
_cell_length_b                   12.0362(7)
_cell_length_c                   40.298(2)
_cell_measurement_reflns_used    5682
_cell_measurement_temperature    150.03(18)
_cell_measurement_theta_max      24.3440
_cell_measurement_theta_min      3.5610
_cell_volume                     14277.9(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      150.03(18)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -54.00   58.00   1.0000   23.0400
omega____ theta____ kappa____ phi______ frames
    -       20.8673    0.0000  -90.0000 112

  2 omega    5.00   61.00   1.0000   23.0400
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -99.0000  150.0000 56

  3 omega   60.00  101.00   1.0000   23.0400
omega____ theta____ kappa____ phi______ frames
    -       20.8673 -178.0000   90.0000 41

  4 omega  -70.00  -45.00   1.0000   23.0400
omega____ theta____ kappa____ phi______ frames
    -      -21.1798 -178.0000  120.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0223149000
_diffrn_orient_matrix_UB_12      0.0194939000
_diffrn_orient_matrix_UB_13      -0.0044011000
_diffrn_orient_matrix_UB_21      -0.0069125000
_diffrn_orient_matrix_UB_22      -0.0547621000
_diffrn_orient_matrix_UB_23      0.0017286000
_diffrn_orient_matrix_UB_31      0.0059342000
_diffrn_orient_matrix_UB_32      0.0095436000
_diffrn_orient_matrix_UB_33      0.0188479000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            28116
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.033
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.459
_exptl_crystal_F_000             6360
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.039
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         14566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0390P)^2^+69.9893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9640
_reflns_number_total             14566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01064d2.cif
_cod_data_source_block           I
_cod_original_cell_volume        14278.0(17)
_cod_database_code               7040200
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C100 H120 N6 Co2 B1 Br2 F48'
_reflns_odcompleteness_completeness 99.65
_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 C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F17A) = Uanis(F16B) = Uanis(F16A) = Uanis(F18B) = Uanis(F18A) =
Uanis(F17B)
3. Others
 Sof(F16B)=Sof(F17B)=Sof(F18B)=1-FVAR(1)
 Sof(F17A)=Sof(F16A)=Sof(F18A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C35(H35A,H35B), C37(H37A,H37B), C36(H36A,H36B)
4.b Aromatic/amide H refined with riding coordinates:
 C68(H68), C58(H58), C44(H44), C40(H40), C10(H10), C21(H21), N3(H3), C48(H48),
 C12(H12), C52(H52), C66(H66), C56(H56), C50(H50), C64(H64), C60(H60), C30(H30),
  C28(H28), C42(H42), C19(H19)
4.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C1(H1A,H1B,H1C), C32(H32A,H32B,H32C), C14(H14A,H14B,
 H14C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C5(H5A,H5B,H5C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              44928
_olex2_submission_special_instructions 'No special instructions were received'