Cobalt-Catalyzed Regioselective Olefin Isomerization Under Kinetic Control.
Liu, Xufang; Zhang, Wei; Wang, Yujie; Zhang, Ze-Xin; Jiao, Lei; Liu, Qiang; Journal of the American Chemical Society 140 (2018) 6873–6882; doi:10.1021/jacs.8b01815

data_4132135
_publ_section_title
;
 Cobalt-Catalyzed Regioselective Olefin Isomerization Under Kinetic
 Control.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6873
_journal_page_last               6882
_journal_paper_doi               10.1021/jacs.8b01815
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C17 H31 Cl2 Co N2 P, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C17.5 H32 Cl3 Co N2 P'
_chemical_formula_weight         466.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                109.275(3)
_cell_angle_beta                 100.010(3)
_cell_angle_gamma                91.118(3)
_cell_formula_units_Z            4
_cell_length_a                   7.8212(3)
_cell_length_b                   15.7879(6)
_cell_length_c                   19.7391(7)
_cell_measurement_reflns_used    5921
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      65.5640
_cell_measurement_theta_min      4.4050
_cell_volume                     2257.98(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -64.00  33.00   1.00    1.00    --  -40.81  38.00 -90.00   97
  2  \w    -49.00 -19.00   1.00    1.00    --  -40.81 125.00   0.00   30
  3  \w    -92.00 -56.00   1.00    1.00    --  -40.81 125.00   0.00   36
  4  \w   -108.00 -16.00   1.00    1.00    --  -40.81 -38.00  90.00   92
  5  \w     94.00 159.00   1.00    4.00    --   89.35 125.00  30.00   65
  6  \w    102.00 159.00   1.00    4.00    --   89.35 125.00  90.00   57
  7  \w     83.00 163.00   1.00    4.00    --   89.35  77.00 150.00   80
  8  \w     84.00 111.00   1.00    4.00    --   89.35 -45.00  90.00   27
  9  \w     82.00 122.00   1.00    4.00    --   89.35 -77.00  60.00   40
 10  \w     53.00 121.00   1.00    4.00    --   89.35-125.00   0.00   68
 11  \w     39.00 118.00   1.00    4.00    --   89.35-125.00 -90.00   79
 12  \w     33.00 120.00   1.00    4.00    --   89.35 -77.00   0.00   87
 13  \w    104.00 161.00   1.00    4.00    --   89.35  45.00-150.00   57
 14  \w     94.00 121.00   1.00    4.00    --   89.35 125.00 -90.00   27
 15  \w     75.00 162.00   1.00    4.00    --   89.35  61.00  90.00   87
 16  \w     25.00  57.00   1.00    4.00    --   89.35 -45.00  90.00   32
 17  \w     13.00  45.00   1.00    4.00    --   89.35 -77.00  60.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0684827000
_diffrn_orient_matrix_UB_12      -0.0823338000
_diffrn_orient_matrix_UB_13      0.0181681000
_diffrn_orient_matrix_UB_21      0.1819927000
_diffrn_orient_matrix_UB_22      0.0507016000
_diffrn_orient_matrix_UB_23      0.0316448000
_diffrn_orient_matrix_UB_31      -0.0497159000
_diffrn_orient_matrix_UB_32      0.0375525000
_diffrn_orient_matrix_UB_33      0.0759179000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14798
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        65.775
_diffrn_reflns_theta_max         65.775
_diffrn_reflns_theta_min         4.425
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0316P)^2^+1.2025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6339
_reflns_number_total             7605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01815_si_004.cif
_cod_data_source_block           fu3pynnptbu3ch2cocl2
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C35 H64 Cl6 Co2 N4 P2'
_cod_original_formula_weight         933.40
_cod_original_formula_moiety         '2(C17 H31 Cl2 Co N2 P), C H2 Cl2'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2257.96(16)
_cod_database_code               4132135
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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.a Ternary CH refined with riding coordinates:
 N00D(H00D), N00E(H00N)
2.b Secondary CH2 refined with riding coordinates:
 C00I(H00P,H00Q), C00J(H00A,H00B), C00M(H00C,H00E), C00Q(H00U,H00V), C00R(H00W,
 H00Y), C00S(H00Z,H), C00W(H00I,H00J), C01B(H01J,H01K), C01D(H01Y,HE)
2.c Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00X(H00X), C00Z(H1AA), C010(H010), C014(H014), C017(H017),
 C019(H019), C01A(H01X)
2.d Idealised Me refined as rotating group:
 C00N(H00R,H00S,H00T), C00T(H00,HA,HB), C00U(H00F,H00G,H00H), C00V(H0AA,HC,HD),
  C00Y(H00K,H00L,H00M), C011(H01O,H01P,H01Q), C012(H01A,H01B,H01C), C013(H01D,
 H01E,H01F), C015(H01R,H01S,H01T), C016(H01U,H01V,H01W), C018(H01G,H01H,H01I),
 C01C(H01L,H01M,H01N)
;
_olex2_date_sample_data_collection 2017-04-19
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.437
_oxdiff_exptl_absorpt_empirical_full_min 0.670