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_7220491
_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
'C66 H82 Br2 Co2 N6 O2, 2(C32 H12 B F24), C2 H4 Cl2'
_chemical_formula_sum            'C132 H110 B2 Br2 Cl2 Co2 F48 N6 O2'
_chemical_formula_weight         3094.45
_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             2014-11-09
_audit_creation_method
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Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
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_audit_update_record
;
2015-03-23 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                77.217(3)
_cell_angle_beta                 76.631(3)
_cell_angle_gamma                85.363(3)
_cell_formula_units_Z            1
_cell_length_a                   12.6292(4)
_cell_length_b                   16.5399(5)
_cell_length_c                   16.5440(6)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    99.90(14)
_cell_measurement_theta_max      27.3192
_cell_measurement_theta_min      2.9730
_cell_volume                     3277.22(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      99.90(14)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_details
;
  1 omega  -58.00   50.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.4693   77.0000 -150.0000 108

  2 omega  -12.00  103.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8755   77.0000  -30.0000 115

  3 omega    9.00   35.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8755   77.0000 -180.0000 26

  4 omega  -11.00  101.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8755   77.0000   90.0000 112
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0397307000
_diffrn_orient_matrix_UB_12      0.0302266000
_diffrn_orient_matrix_UB_13      -0.0203736000
_diffrn_orient_matrix_UB_21      0.0282994000
_diffrn_orient_matrix_UB_22      -0.0136616000
_diffrn_orient_matrix_UB_23      0.0331909000
_diffrn_orient_matrix_UB_31      0.0309256000
_diffrn_orient_matrix_UB_32      -0.0289019000
_diffrn_orient_matrix_UB_33      -0.0226680000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19773
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.379
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.624
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         12632
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0919P)^2^+4.6358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10227
_reflns_number_total             12632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra06792h2.cif
_cod_data_source_block           ofm4
_cod_original_cell_volume        3277.2(2)
_cod_database_code               7220491
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C132 H106 N6 O2 F48 Cl2 Co2 Br2 B2'
_chemical_oxdiff_usercomment     'brown crystal 0.1 0.1 0.'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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
 F23A-C65 \\sim C65-F22A \\sim F24A-C65 \\sim C65-F23A \\sim F22A-C65 \\sim
C65-F24A
 with sigma of 0.02
 F24A-F23A \\sim F23A-F22A \\sim F23A-F22A \\sim F22A-F24A \\sim F22A-F24A
\\sim F24A-F23A
 with sigma of 0.02
 F24B-C65 \\sim C65-F23B \\sim F23B-C65 \\sim C65-F22B \\sim F22B-C65 \\sim
C65-F24B
 with sigma of 0.02
 F24B-F23B \\sim F23B-F22B \\sim F23B-F22B \\sim F22B-F24B \\sim F22B-F24B
\\sim F24B-F23B
 with sigma of 0.02
 F17B-C57 \\sim C57-F16B \\sim F16B-C57 \\sim C57-F18B \\sim F18B-C57 \\sim
C57-F17B
 with sigma of 0.02
 F17B-F16B \\sim F16B-F18B \\sim F16B-F18B \\sim F18B-F17B \\sim F18B-F17B
\\sim F17B-F16B
 with sigma of 0.02
 F17A-C57 \\sim C57-F16A \\sim F16A-C57 \\sim C57-F18A \\sim F18A-C57 \\sim
C57-F17A
 with sigma of 0.02
 F17A-F16A \\sim F16A-F18A \\sim F16A-F18A \\sim F18A-F17A \\sim F18A-F17A
\\sim F17A-F16A
 with sigma of 0.02
 F13B-C56 \\sim C56-F15B \\sim F15B-C56 \\sim C56-F14B \\sim F14B-C56 \\sim
C56-F13B
 with sigma of 0.02
 F13B-F15B \\sim F15B-F14B \\sim F15B-F14B \\sim F14B-F13B \\sim F14B-F13B
\\sim F13B-F15B
 with sigma of 0.02
 F13A-C56 \\sim C56-F15A \\sim F15A-C56 \\sim C56-F14A \\sim F14A-C56 \\sim
C56-F13A
 with sigma of 0.02
 F13A-F15A \\sim F15A-F14A \\sim F15A-F14A \\sim F14A-F13A \\sim F14A-F13A
\\sim F13A-F15A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F24A) = Uanis(F24B) = Uanis(F23A) = Uanis(F23B) = Uanis(F22A) =
Uanis(F22B) = Uanis(C65)
Uanis(F14B) = Uanis(F14A) = Uanis(F13A) = Uanis(F13B) = Uanis(C56) =
Uanis(F15A) = Uanis(F15B)
4. Rigid body (RIGU) restrains
 F18A, F18B, C57, F17A, F17B, F16A, F16B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F24B)=Sof(F23B)=Sof(F22B)=1-FVAR(1)
 Sof(F22A)=Sof(F24A)=Sof(F23A)=FVAR(1)
 Sof(F17A)=Sof(F18A)=Sof(F16A)=1-FVAR(2)
 Sof(F17B)=Sof(F18B)=Sof(F16B)=FVAR(2)
 Sof(F14A)=Sof(F13A)=Sof(F15A)=1-FVAR(3)
 Sof(F15B)=Sof(F13B)=Sof(F14B)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C3(H3)
6.b Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B)
6.c Aromatic/amide H refined with riding coordinates:
 C55(H55), C39(H39), C43(H43), C47(H47), C63(H63), C53(H53), C35(H35),
 C51(H51), C59(H59), C61(H61), C37(H37), C14(H14), C32(H32), C21(H21), C30(H30),
  C45(H45), C13(H13), C29(H29), C31(H31), C15(H15), C23(H23), C22(H22)
6.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C33(H33A,H33B,H33C), C10(H10A,H10B,H10C),
 C1(H1A,H1B,H1C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C9(H9A,H9B,H9C),
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              63763
_olex2_submission_special_instructions 'No special instructions were received'