Computational Transition-State Design Provides Experimentally Verified Cr(P,N) Catalysts for Control of Ethylene Trimerization and Tetramerization
Kwon, Doo-Hyun; Fuller, Jack T.; Kilgore, Uriah J.; Sydora, Orson L.; Bischof, Steven M.; Ess, Daniel H.; ACS Catalysis 8 (2018) 1138–; doi:10.1021/acscatal.7b04026

data_4514356
_publ_section_title
;
 Computational Transition-State Design Provides Experimentally Verified
 Cr(P,N) Catalysts for Control of Ethylene Trimerization and
 Tetramerization
;
_journal_issue                   2
_journal_name_full               'ACS Catalysis'
_journal_page_first              1138
_journal_paper_doi               10.1021/acscatal.7b04026
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C18 H37 Cl4 Cr Li N2 O2 P'
_chemical_formula_sum            'C18 H37 Cl4 Cr Li N2 O2 P'
_chemical_formula_weight         545.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-06-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.537(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0101(4)
_cell_length_b                   19.2905(10)
_cell_length_c                   14.2617(7)
_cell_measurement_reflns_used    3178
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.340
_cell_measurement_theta_min      4.585
_cell_volume                     2578.9(2)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_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_temperature      100.0
_diffrn_detector                 'Bruker Platinum135 CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Platinum135'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17679
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         68.334
_diffrn_reflns_theta_min         4.026
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Rigaku MicroMax-007HF'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.181
_exptl_absorpt_correction_T_max  0.3201
_exptl_absorpt_correction_T_min  0.1886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1018 before and 0.0711 after correction. The Ratio of minimum to maximum transmission is 0.5892. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0864P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3170
_reflns_number_total             4727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b04026_si_002.cif
_cod_data_source_block           Chevron34
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_colour_primary' value 'Blue' changed to 'blue'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4514356.cif.
;
_cod_database_code               4514356
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.265
_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:
 C5(H5), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
  C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              72845
_shelx_hkl_checksum              70566
_olex2_submission_special_instructions 'No special instructions were received'