Alpha and beta diimine cobalt complexes in isoprene polymerization: a comparative study
Alnajrani, Mohammed; Alshmimri, Sultan A.; Alsager, Omar A.; RSC Adv.  (2016) –; doi:10.1039/C6RA23308B

data_7227215
_publ_section_title
;
 Alpha and beta diimine cobalt complexes in isoprene polymerization: a
 comparative study
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA23308B
_journal_year                    2016
_chemical_formula_moiety         'C29 H42 Br2 Co N2, C H2 Cl2'
_chemical_formula_sum            'C30 H44 Br2 Cl2 Co N2'
_chemical_formula_weight         722.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2016-09-18 deposited with the CCDC.
2016-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.005(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4172(12)
_cell_length_b                   7.9998(3)
_cell_length_c                   21.5000(11)
_cell_measurement_reflns_used    4147
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8360
_cell_measurement_theta_min      3.1630
_cell_volume                     3278.3(3)
_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      293(2)
_diffrn_detector_area_resol_mean 16.1428
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   21.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  -99.0000    0.0000 40

  2 omega   48.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  178.0000  120.0000 29

  3 omega   70.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8673  178.0000   30.0000 26

  4 omega  -87.00    0.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   19.0000 -150.0000 87

  5 omega  -46.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   37.0000 -120.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0278204000
_diffrn_orient_matrix_UB_12      0.0246978000
_diffrn_orient_matrix_UB_13      -0.0246967000
_diffrn_orient_matrix_UB_21      -0.0204481000
_diffrn_orient_matrix_UB_22      0.0222305000
_diffrn_orient_matrix_UB_23      0.0227459000
_diffrn_orient_matrix_UB_31      0.0139176000
_diffrn_orient_matrix_UB_32      0.0822019000
_diffrn_orient_matrix_UB_33      0.0012977000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15496
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.142
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72753
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0243P)^2^+4.6367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4834
_reflns_number_total             6695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra23308b2.cif
_cod_data_source_block           B
_cod_database_code               7227215
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C29H42N2CoBr2
_reflns_odcompleteness_completeness 99.75
_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.a Ternary CH refined with riding coordinates:
 C12(H12), C27(H27), C15(H15), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C22(H22), C21(H21), C8(H8), C9(H9), C10(H10)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C),
 C28(H28A,H28B,H28C), C16(H16A,H16B,H16C), C26(H26A,H26B,H26C), C25(H25A,H25B,
 H25C), C29(H29A,H29B,H29C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              22956
_olex2_submission_special_instructions 'No special instructions were received'