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_7220492
_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
'C58 H58 Br2 Co2 F8 N6 O2, 2(C32 H12 B F24), C0.52 H1.91 Cl2'
_chemical_formula_sum            'C122 H82 B2 Br2 Cl2 Co2 F56 N6 O2'
_chemical_formula_weight         3098.13
_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     direct
_audit_creation_date             2014-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-03-23 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                77.298(4)
_cell_angle_beta                 83.896(4)
_cell_angle_gamma                78.943(4)
_cell_formula_units_Z            1
_cell_length_a                   12.3778(6)
_cell_length_b                   16.0019(7)
_cell_length_c                   17.1622(8)
_cell_measurement_reflns_used    4787
_cell_measurement_temperature    150.01(11)
_cell_measurement_theta_max      23.6580
_cell_measurement_theta_min      3.7200
_cell_volume                     3247.2(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
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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    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(11)
_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 0.998
_diffrn_measurement_details
;
  1 omega   -2.00   74.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       23.9100   57.0000    0.0000 76

  2 omega   -5.00   90.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       23.9100   77.0000  120.0000 95

  3 omega  -16.00   17.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.8162  -99.0000    0.0000 33

  4 omega  -18.00   14.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.8162  -99.0000  150.0000 32

  5 omega  -85.00    8.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.8162  -37.0000    0.0000 93

  6 omega   33.00   80.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       23.9100   37.0000 -150.0000 47

  7 omega  -51.00   50.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.8162   77.0000 -120.0000 101
;
_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      0.0141190000
_diffrn_orient_matrix_UB_12      -0.0417143000
_diffrn_orient_matrix_UB_13      -0.0098320000
_diffrn_orient_matrix_UB_21      -0.0405599000
_diffrn_orient_matrix_UB_22      -0.0152317000
_diffrn_orient_matrix_UB_23      0.0292593000
_diffrn_orient_matrix_UB_31      -0.0397505000
_diffrn_orient_matrix_UB_32      0.0125172000
_diffrn_orient_matrix_UB_33      -0.0291582000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.1364
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24548
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.326
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74628
_exptl_absorpt_correction_type   analytical
_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    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.702
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         13245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1702
_refine_ls_R_factor_gt           0.0896
_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^)+(0.1284P)^2^+3.5445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6945
_reflns_number_total             13245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra06792h2.cif
_cod_data_source_block           afm26
_cod_database_code               7220492
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C100H100O2N6Co2Br2B2F56
_reflns_odcompleteness_completeness 99.77
_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. Uiso/Uaniso restraints and constraints
Uanis(F16A) = Uanis(F16B) = Uanis(F14A) = Uanis(F14B) = Uanis(F15A) =
Uanis(F15B)
Uanis(F14B) = Uanis(F14A) = Uanis(F16B) = Uanis(F16A) = Uanis(F15B) =
Uanis(F15A)
Uanis(F26B) = Uanis(F27B) = Uanis(F28A) = Uanis(F28B)
Uanis(F20A) = Uanis(F20B) = Uanis(F21A) = Uanis(F21B) = Uanis(F22B) =
Uanis(F22B)
Uanis(F7B) = Uanis(F7A)
Uanis(F6B) = Uanis(F6A)
Uanis(F6) = Uanis(F18) = Uanis(F15) = Uanis(F14) = Uanis(F16) = Uanis(F7)
3. Others
 Sof(F16A)=Sof(F15A)=Sof(F14A)=1-FVAR(1)
 Sof(F16B)=Sof(F15B)=Sof(F14B)=FVAR(1)
 Sof(F27A)=Sof(F26A)=Sof(F28A)=1-FVAR(2)
 Sof(F26B)=Sof(F28B)=Sof(F27B)=FVAR(2)
 Sof(F22A)=Sof(F20A)=Sof(F21A)=1-FVAR(3)
 Sof(F21B)=Sof(F22B)=Sof(F20B)=FVAR(3)
 Sof(F7A)=1-FVAR(4)
 Sof(F7B)=FVAR(4)
 Sof(F6B)=1-FVAR(5)
 Sof(F6A)=FVAR(5)
 Sof(F7)=Sof(F14)=Sof(F18)=1-FVAR(6)
 Sof(F6)=Sof(F15)=Sof(F16)=FVAR(6)
4.a Ternary CH refined with riding coordinates:
 C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB)
4.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C55(H55), C51(H51), C31(H31), C59(H59), C43(H43), C41(H41),
 C33(H33), C47(H47), C39(H39), C49(H49), C15(H15), C13(H13), C14(H14), C57(H57),
  C28(H28), C27(H27), C25(H25), C21(H21), C26(H26), C19(H19), C20(H20)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C29(H29A,H29B,H29C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              36494
_olex2_submission_special_instructions 'No special instructions were received'