Catalytic Enantioselective Hetero-dimerization of Acrylates and 1,3-Dienes.
Jing, Stanley M.; Balasanthiran, Vagulejan; Pagar, Vinayak; Gallucci, Judith C.; RajanBabu, T. V.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10055

data_4126764
_publ_section_title
;
 Catalytic Enantioselective Hetero-dimerization of Acrylates and
 1,3-Dienes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10055
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C81 H78 Br2 Co2 P6, 3(C4 H8 O)'
_chemical_formula_sum            'C93 H102 Br2 Co2 O3 P6'
_chemical_formula_weight         1731.24
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2017-08-31T10:54:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1093(5)
_cell_length_b                   21.7148(6)
_cell_length_c                   23.9709(6)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.42
_cell_measurement_theta_min      2.33
_cell_measurement_wavelength     0.71073
_cell_volume                     9946.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa APEXII CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60864
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.216
_diffrn_reflns_theta_max         25.216
_diffrn_reflns_theta_min         1.363
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker AXS )'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
TITL shelx     P 21 21 21   R = 0.07
CELL   19.1093   21.7148   23.9709     90.00     90.00     90.00
SPGR P212121
C101 0.840 0.773 0.163 !       3.31 eA-3
C102 0.808 0.820 0.983 !       3.08 eA-3
C103 0.160 0.321 0.295 !       3.07 eA-3
C104 0.024 0.820 0.984 !       3.04 eA-3
C105 0.075 0.312 0.298 !       3.00 eA-3
C106 0.051 0.290 0.329 !       2.93 eA-3
C107 0.599 0.750 0.061 !       2.91 eA-3
C108 0.467 0.224 0.437 !       2.85 eA-3
C109 0.887 0.757 0.140 !       2.81 eA-3
C110 0.310 0.630 0.092 !       2.79 eA-3
C111 0.417 0.214 0.514 !       2.77 eA-3
C112 0.153 0.329 0.563 !       2.66 eA-3
C113 0.562 0.698 0.072 !       2.54 eA-3
C114 0.119 0.756 0.001 !       2.46 eA-3
C115 0.718 0.095 0.444 !       2.40 eA-3
C116 0.912 0.766 0.111 !       2.35 eA-3
C117 0.724 0.117 0.485 !       2.21 eA-3
C118 0.864 0.104 0.603 !       1.54 eA-3
C119 0.857 0.038 0.603 !       1.39 eA-3
C120 0.310 0.381 0.407 !       1.34 eA-3
C121 0.805 0.072 0.609 !       1.26 eA-3
C122 0.680 0.860 0.124 !       1.19 eA-3
Q123 0.175 0.603 0.861 !       1.07 eA-3
C124 0.126 0.313 0.382 !       0.98 eA-3
Q125 0.296 0.377 0.330 !       0.94 eA-3
C126 0.828 0.748 0.985 !       0.90 eA-3
C127 0.802 0.031 0.625 !       0.88 eA-3
C128 0.863 0.875 0.958 !       0.86 eA-3
C129 0.085 0.291 0.519 !       0.82 eA-3
C130 0.611 0.135 0.391 !       0.82 eA-3
Q131 0.153 0.407 0.608 !       0.81 eA-3
Q132 0.262 0.804 0.414 !       0.77 eA-3
C133 0.140 0.201 0.353 !       0.76 eA-3
C134 0.878 0.833-0.001 !       0.75 eA-3
C135 0.228 0.266 0.526 !       0.74 eA-3
Q136 0.027 0.352 0.351 !       0.74 eA-3
C137 0.054 0.281 0.251 !       0.74 eA-3
Q138 0.605 0.353 0.774 !       0.74 eA-3
C139 0.399 0.801 0.845 !       0.73 eA-3
C140 0.275 0.336 0.562 !       0.73 eA-3
C141 0.912 0.856 0.960 !       0.72 eA-3
C142 0.360 0.743 0.055 !       0.71 eA-3
Q143 0.263 0.806 0.368 !       0.71 eA-3
C144 0.279 0.331 0.458 !       0.69 eA-3
Q145 0.122 0.228 0.305 !       0.68 eA-3
C146 0.322 0.705 0.962 !       0.67 eA-3
Q147 0.142 0.208 0.428 !       0.65 eA-3
Q148 0.414 0.892 0.717 !       0.65 eA-3
Q149 0.999 0.180 0.554 !       0.65 eA-3
Q150 0.905 0.945 0.766 !       0.64 eA-3
C151 0.671 0.262 0.599 !       0.64 eA-3
C152 0.528 0.694 0.930 !       0.63 eA-3
C153 0.233 0.596 0.930 !       0.63 eA-3
C154 0.185 0.728 0.924 !       0.62 eA-3
Q155 0.838 0.861 0.142 !       0.62 eA-3
Q156 0.614 0.273 0.104 !       0.61 eA-3
C157 0.294 0.364 0.494 !       0.61 eA-3
Q158 0.606 0.359 0.744 !       0.61 eA-3
C159 0.194 0.259 0.486 !       0.61 eA-3
Q160 0.857 0.290 0.438 !       0.60 eA-3
Q161 0.096 0.265 0.907 !       0.60 eA-3
Q162 0.724 0.943 0.014 !       0.60 eA-3
C163 0.878 0.052 0.633 !       0.60 eA-3
C164 0.885 0.158 0.586 !       0.58 eA-3
C165 0.076 0.335 0.581 !       0.58 eA-3
Q166 0.378 0.895 0.726 !       0.58 eA-3
Q167 0.595 0.821 0.057 !       0.58 eA-3
C168 0.458 0.656 0.018 !       0.57 eA-3
Q169 0.242 0.239 0.875 !       0.57 eA-3
Q170 0.670 0.452 0.796 !       0.57 eA-3
C171 0.680 0.162 0.569 !       0.57 eA-3
Q172 0.412 0.429 0.399 !       0.56 eA-3
Q173 0.171 0.046 0.250 !       0.56 eA-3
C174 0.795 0.079 0.414 !       0.56 eA-3
Q175 0.357 0.406 0.467 !       0.56 eA-3
Q176 0.021 0.322 0.271 !       0.56 eA-3
Q177 0.491 0.237 0.382 !       0.56 eA-3
Q178 0.964 0.742 0.892 !       0.56 eA-3
Q179 0.262 0.695 0.585 !       0.55 eA-3
C180 0.856 0.759 0.025 !       0.54 eA-3
Q181 0.110 0.868 0.305 !       0.54 eA-3
Q182 0.653 0.179 0.766 !       0.53 eA-3
C183 0.644 0.814 0.064 !       0.53 eA-3
Q184 0.361 0.636 0.900 !       0.53 eA-3
C185 0.024 0.251 0.493 !       0.53 eA-3
Q186 0.193 0.998 0.280 !       0.53 eA-3
C187 0.680 0.270 0.555 !       0.53 eA-3
Q188 0.031 0.234 0.258 !       0.53 eA-3
Q189 0.241 0.727 0.799 !       0.52 eA-3
C190 0.813 0.118 0.547 !       0.52 eA-3
C191 0.486 0.728 0.936 !       0.51 eA-3
Q192 0.804 0.076 0.742 !       0.51 eA-3
Q193 0.600 0.203 0.763 !       0.51 eA-3
Q194 0.075 0.530 0.873 !       0.51 eA-3
Q195 0.383 0.130 0.488 !       0.51 eA-3
Q196 0.135 0.183 0.383 !       0.51 eA-3
Q197 0.616 0.258 0.406 !       0.51 eA-3
Q198 0.617 0.608 0.078 !       0.51 eA-3
;
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 5353 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     955
_refine_ls_number_reflns         17805
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                13907
_reflns_number_total             17805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10055_si_003.cif
_cod_data_source_block           RajanBabu2080
_cod_database_code               4126764
_platon_squeeze_void_probe_radius 1.20