The behaviour of β-triketimine cobalt complexes in the polymerization of isoprene
Mair, F. S.; Alnajrani, Mohammed Nasser; RSC Adv.  (2015) –; doi:10.1039/C5RA06792H

data_7220489
_publ_section_title
;
 The behaviour of \b-triketimine cobalt complexes in the polymerization of
 isoprene
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA06792H
_journal_year                    2015
_chemical_formula_moiety
'C56 H62 Br1.93 Co2 N6, 2(C32 H12 B F24), C2 H4 Cl2'
_chemical_formula_sum            'C122 H90 B2 Br1.93 Cl2 Co2 F48 N6'
_chemical_formula_weight         2916.65
_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
_audit_creation_date             2014-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-03-22 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                75.314(4)
_cell_angle_beta                 83.402(4)
_cell_angle_gamma                71.836(4)
_cell_formula_units_Z            1
_cell_length_a                   12.8325(6)
_cell_length_b                   15.0886(7)
_cell_length_c                   17.1355(7)
_cell_measurement_reflns_used    7959
_cell_measurement_temperature    150.03(16)
_cell_measurement_theta_max      28.3680
_cell_measurement_theta_min      3.2930
_cell_volume                     3047.2(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      150.03(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega  -77.00   45.00   1.0000   44.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7110   19.0000  -90.0000 122

  2 omega   19.00   66.00   1.0000   44.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -99.0000 -150.0000 47

  3 omega  -12.00   94.00   1.0000   44.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   77.0000   90.0000 106

  4 omega   34.00  103.00   1.0000   44.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360 -178.0000   60.0000 69
;
_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      0.0242923000
_diffrn_orient_matrix_UB_12      -0.0427642000
_diffrn_orient_matrix_UB_13      -0.0136912000
_diffrn_orient_matrix_UB_21      -0.0525704000
_diffrn_orient_matrix_UB_22      -0.0000867000
_diffrn_orient_matrix_UB_23      -0.0089575000
_diffrn_orient_matrix_UB_31      0.0059533000
_diffrn_orient_matrix_UB_32      0.0275038000
_diffrn_orient_matrix_UB_33      -0.0395756000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_laue_measured_fraction_full 0.986
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_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18523
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.137
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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    1.589
_exptl_crystal_F_000             1462
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.286
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         12273
_refine_ls_number_restraints     371
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0960P)^2^+6.6540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.1967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9596
_reflns_number_total             12273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra06792h2.cif
_cod_data_source_block           afm16
_cod_original_cell_volume        3047.2(2)
_cod_database_code               7220489
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C100H100N6Co2Br2B2F48
_reflns_odcompleteness_completeness 98.56
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C12
 1.5 with sigma of 0.02
 C13A-C12A
 1.5 with sigma of 0.02
 C19-C20
 1.4 with sigma of 0.02
 Cl1-C1S
 1.7 with sigma of 0.02
 F48A-C59 \\sim C59-F34A \\sim F34A-C59 \\sim C59-F24A \\sim F24A-C59 \\sim
C59-F48A
 with sigma of 0.02
 F48A-F24A \\sim F24A-F34A \\sim F24A-F34A \\sim F34A-F48A \\sim F34A-F48A
\\sim F48A-F24A
 with sigma of 0.02
 F30A-C43 \\sim C43-F40A
 with sigma of 0.02
 F40A-C43 \\sim C43-F12A
 with sigma of 0.02
 F12A-C43 \\sim C43-F30A
 with sigma of 0.02
 C12A-C13A \\sim C13-C12
 with sigma of 0.02
 C20-C19 \\sim C20A-C19A
 with sigma of 0.02
 F27-C34 \\sim C34-F9 \\sim F9-C34 \\sim C34-F15 \\sim F15-C34 \\sim C34-F27
\\sim F27A-C34 \\sim C34-F15A
 \\sim F15A-C34 \\sim C34-F9A \\sim F9A-C34 \\sim C34-F27A
 with sigma of 0.02
3. Rigid bond restraints
 Cl1, C1S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Br1C \\sim Br1B \\sim Br1A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C13 \\sim C13A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C20 \\sim C20A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(Cl1) \\sim Ueq, Uanis(C1S) \\sim Ueq, : with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C13) = Uanis(C13A)
Uanis(C20) = Uanis(C20A)
Uanis(F9) = Uanis(F15A) = Uanis(F15) = Uanis(F27A) = Uanis(F27) = Uanis(F9A)
5. Rigid body (RIGU) restrains
 Br1C, Br1A, Br1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F24, F34, F48, C59, F48A, F24A, F34A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F12, F30, F40, C43, F40A, F12A, F30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C9, C10, C11, C12, C7A, C8A, C9A, C10A, C11A, C12A, C13A, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1A, C20, C18, C19, C14, C16, C17, C14A, C16A, C17A, C18A, C19A, C20A, N1B,
 C15, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F9, F15, F27, C34, F9A, F27A, F15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1S, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Br1A)]+1*[Sof(Br1B)]+1*[Sof(Br1C)]=1 with esd of 0.01
 Sof(N1A)=Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=
 Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(C20A)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=1-FVAR(1)
 Sof(N1B)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(C14)=Sof(C15)=Sof(H15)=Sof(C16)=
 Sof(H16)=Sof(C17)=Sof(H17)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=
 Sof(H11A)=Sof(C12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(5)
 Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(5)
 Sof(F24A)=Sof(F34A)=Sof(F48A)=1-FVAR(6)
 Sof(F24)=Sof(F34)=Sof(F48)=FVAR(6)
 Sof(F12A)=Sof(F30A)=Sof(F40A)=1-FVAR(7)
 Sof(F12)=Sof(F30)=Sof(F40)=FVAR(7)
 Sof(F9A)=Sof(F15A)=Sof(F27A)=1-FVAR(8)
 Sof(F9)=Sof(F15)=Sof(F27)=FVAR(8)
7.a Ternary CH refined with riding coordinates:
 C3(H3)
7.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
7.c Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C13A(H13D,H13E,H13F), C20A(H20D,
 H20E,H20F)
7.d Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C8(H8), C9(H9), C10(H10), C11(H11),
 C18(H18), C15(H15), C16(H16), C17(H17), C8A(H8A), C9A(H9A), C10A(H10A),
 C11A(H11A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C29(H29), C31(H31),
  C33(H33), C37(H37), C39(H39), C41(H41), C45(H45), C47(H47), C49(H49),
 C53(H53), C55(H55), C57(H57)
7.e Fitted hexagon refined as free rotating group:
 C7(C8,C9,C10,C11,C12), C18(C19,C14,C15,C16,C17), C7A(C8A,C9A,C10A,C11A,C12A),
 C14A(C15A,C16A,C17A,C18A,C19A)
7.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2A(H2AA,H2AB,H2AC), C6(H6A,H6B,H6C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              3925
_olex2_submission_special_instructions 'No special instructions were received'