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_4132137
_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         'C15 H27 Cl2 Co N2 P'
_chemical_formula_sum            'C15 H27 Cl2 Co N2 P'
_chemical_formula_weight         396.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6705(5)
_cell_length_b                   8.1102(2)
_cell_length_c                   27.7803(7)
_cell_measurement_reflns_used    4950
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.0950
_cell_measurement_theta_min      5.5320
_cell_volume                     3755.93(17)
_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)'
_computing_structure_solution    'ShelXT (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     40.00  95.00   1.00    1.00    --   40.81-125.00  60.00   55
  2  \w     46.00  72.00   1.00    5.00    --  100.91 -61.00   0.00   26
  3  \w     90.00 130.00   1.00    5.00    --  100.91 -61.00   0.00   40
  4  \w     74.00 104.00   1.00    5.00    --  100.91 -95.00  90.00   30
  5  \w     27.00  97.00   1.00    5.00    --  100.91 -30.00 -60.00   70
  6  \w     31.00 130.00   1.00    5.00    --  100.91 -77.00-120.00   99
  7  \w     19.00  58.00   1.00    5.00    --  100.91 -95.00  90.00   39
  8  \w     20.00  93.00   1.00    5.00    --  100.91 -95.00-180.00   73
  9  \w    146.00 174.00   1.00    5.00    --  100.91 125.00-180.00   28
 10  \w   -117.00   2.00   1.00    1.00    --  -40.81   0.00  90.00  119
;
_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      0.0917771000
_diffrn_orient_matrix_UB_12      -0.0217250000
_diffrn_orient_matrix_UB_13      -0.0009309000
_diffrn_orient_matrix_UB_21      0.0088506000
_diffrn_orient_matrix_UB_22      0.1694153000
_diffrn_orient_matrix_UB_23      -0.0245019000
_diffrn_orient_matrix_UB_31      0.0060402000
_diffrn_orient_matrix_UB_32      0.0829537000
_diffrn_orient_matrix_UB_33      0.0497724000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10990
_diffrn_reflns_point_group_measured_fraction_full 0.697
_diffrn_reflns_point_group_measured_fraction_max 0.697
_diffrn_reflns_theta_full        59.999
_diffrn_reflns_theta_max         59.999
_diffrn_reflns_theta_min         5.307
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05619
_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    1.401
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.560
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.219(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         3887
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1408P)^2^+7.8706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.1954
_reflns_Friedel_coverage         0.363
_reflns_Friedel_fraction_full    0.380
_reflns_Friedel_fraction_max     0.380
_reflns_number_gt                3644
_reflns_number_total             3887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01815_si_003.cif
_cod_data_source_block           fu3pynnp3ch2iprcocl2
_cod_database_code               4132137
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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:
 N00B(H00B), N00C(H00N), C00M(H00R), C00T(H0AA), C00Y(H00Y), C012(H012)
2.b Secondary CH2 refined with riding coordinates:
 C00E(H00P,H00Q), C00J(H00A,H00C), C00L(H00D,H00E), C00O(H00T,H00U), C00S(H00H,
 H00J), C00V(H2AA,HB), C00X(H3AA,HC), C011(H01A,H01B)
2.c Aromatic/amide H refined with riding coordinates:
 C00D(H00O), C00F(H00F), C00G(H00G), C00I(H00I), C00N(H00S), C00Q(H00Z),
 C00U(H1AA), C010(H010)
2.d Idealised Me refined as rotating group:
 C00P(H00V,H00W,H00X), C00R(H00,H,HA), C00W(H00K,H00L,H00M), C00Z(H4AA,HD,HE),
 C013(H01L,H01M,H01N), C014(H01C,H01D,H01E), C015(H01F,H01G,H01H), C016(H01I,
 H01J,H01K)
;
_olex2_date_sample_data_collection 2017-04-11
_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 12.498
_oxdiff_exptl_absorpt_empirical_full_min 0.566