Phosphanyl Methanimine (PCN) Ligands for the Selective Trimerization/Tetramerization of Ethylene with Chromium
Radcliffe, James E.; Batsanov, Andrei S.; Smith, David M.; Scott, John A.; Dyer, Philip W.; Hanton, Martin J.; ACS Catalysis 5 (2015) 7095–; doi:10.1021/acscatal.5b02106

data_4513678
_publ_section_title
;
 Phosphanyl Methanimine (PCN) Ligands for the Selective
 Trimerization/Tetramerization of Ethylene with Chromium
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              7095
_journal_paper_doi               10.1021/acscatal.5b02106
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C29 H36 Cr N O4 P'
_chemical_formula_sum            'C29 H36 Cr N O4 P'
_chemical_formula_weight         545.56
_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   mixed
_audit_creation_date             2015-09-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.4771(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.79138(14)
_cell_length_b                   14.69577(18)
_cell_length_c                   16.3394(2)
_cell_measurement_reflns_used    20241
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.1770
_cell_measurement_theta_min      1.9110
_cell_volume                     2822.71(6)
_computing_cell_refinement
;CrysAlisPro, Agilent Technologies, Version 1.171.37.31 
(release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;CrysAlisPro, Agilent Technologies, Version 1.171.37.31 
(release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;CrysAlisPro, Agilent Technologies, Version 1.171.37.31 
(release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
'ShelXL 2014/7 multi-CPU version (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.15
_diffrn_detector_type            'Sapphire3 CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
;
  1 omega  -99.00  -35.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.7883 -178.0000   30.0000 128

  2 omega   35.00  100.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5695  178.0000  150.0000 130

  3 omega  -12.00   98.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5695   19.0000   30.0000 220

  4 omega  -12.00   98.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5695   19.0000  -60.0000 220

  5 omega  -95.00  -21.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.7883  -38.0000    0.0000 148

  6 omega  -16.00   23.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5695  101.0000   12.3954 78

  7 omega    1.00   85.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5695 -132.0000  -45.2488 168

  8 omega   -3.00   95.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5695   77.0000  150.0000 196

  9 omega  -47.00   63.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5695  -19.0000 -150.0000 220
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent Technologies, Gemini S Ultra kappa-diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0384623000
_diffrn_orient_matrix_UB_12      -0.0041404000
_diffrn_orient_matrix_UB_13      0.0354124000
_diffrn_orient_matrix_UB_21      0.0254654000
_diffrn_orient_matrix_UB_22      -0.0382468000
_diffrn_orient_matrix_UB_23      -0.0176867000
_diffrn_orient_matrix_UB_31      0.0388603000
_diffrn_orient_matrix_UB_32      0.0291381000
_diffrn_orient_matrix_UB_33      -0.0181937000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53488
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.472
_diffrn_reflns_theta_min         1.866
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.6323
_exptl_crystal_size_mid          0.4741
_exptl_crystal_size_min          0.3061
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         9401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0420P)^2^+1.1300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8325
_reflns_number_total             9401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs5b02106_si_003.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 4513677--4513678.cif.'
_cod_original_cell_volume        2822.70(6)
_cod_database_code               4513678
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Uiso(H7A)=Uiso(H7B)=Uiso(H7C)=FVAR(1)
 Uiso(H8A)=Uiso(H8B)=Uiso(H8C)=FVAR(2)
 Uiso(H10A)=Uiso(H10B)=Uiso(H10C)=FVAR(3)
 Uiso(H11A)=Uiso(H11B)=Uiso(H11C)=FVAR(4)
 Uiso(H26A)=Uiso(H26B)=Uiso(H26C)=FVAR(5)
 Uiso(H27A)=Uiso(H27B)=Uiso(H27C)=FVAR(6)
 Uiso(H29A)=Uiso(H29B)=Uiso(H29C)=FVAR(7)
 Uiso(H30A)=Uiso(H30B)=Uiso(H30C)=FVAR(8)
3.a Riding coordinates:
 C6(H6), C9(H9), C25(H25), C28(H28)
3.b Rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
3.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'