Benzylene-linked [PNP] scaffolds and their cyclometalated zirconium and hafnium complexes
Sietzen, Malte; Batke, Sonja; Antoni, Patrick W.; Wadepohl, Hubert; Ballmann, Joachim; Dalton Trans.  (2017) –; doi:10.1039/C7DT00413C

data_7042699
_publ_section_title
;
 Benzylene-linked [PNP] scaffolds and their cyclometalated zirconium and
 hafnium complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00413C
_journal_year                    2017
_chemical_formula_moiety         'C38 H33 N P2'
_chemical_formula_sum            'C38 H33 N P2'
_chemical_formula_weight         565.59
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_sb17
_audit_creation_date
;
'Wed Oct 29 13:37:29 2014'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                111.4620(12)
_cell_angle_beta                 107.2399(11)
_cell_angle_gamma                96.1928(10)
_cell_formula_units_Z            2
_cell_length_a                   10.66534(12)
_cell_length_b                   12.26799(17)
_cell_length_c                   13.52930(18)
_cell_measurement_reflns_used    42383
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.7950
_cell_measurement_theta_min      3.7870
_cell_volume                     1526.14(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -46.00   51.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  -35.1244 194

  2 omega  -10.00   81.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000   90.0000 182

  3 omega   -6.00   88.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000 -120.0000 188

  4 omega  -50.00  -11.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000    0.0000 78

  5 omega   -2.00   82.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000    0.0000 168

  6 omega    0.00   38.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000 -150.0000 76

  7 omega  -51.00   48.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000   60.0000 198

  8 omega  -45.00  -19.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -150.0000 52

  9 omega   21.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -150.0000 56

 10 omega  -46.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -120.0000 190

 11 omega    6.00   33.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -38.0000   30.0000 54

 12 omega  -45.00   51.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  133.9178 192

 13 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000   60.0000 180

 14 omega  -25.00   92.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   19.0000   90.0000 234

 15 omega   -3.00   88.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000 -150.0000 182

 16 omega   -3.00   88.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000  -30.0000 182

 17 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000 -120.0000 180

 18 omega  -11.00   89.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000   60.0000 200

 19 omega  -51.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000   90.0000 200

 20 omega  -54.00   44.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -38.0000  -30.0000 196

 21 omega  -51.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -120.0000 200

 22 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000  150.0000 180

 23 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000  -90.0000 180

 24 omega  -46.00   51.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  -35.1244 194

 25 omega  -51.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000 -150.0000 200

 26 omega  -51.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000    0.0000 200

 27 omega  -54.00   92.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505    0.0000    0.0000 292

 28 omega  -54.00   92.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505    0.0000  120.0000 292

 29 omega  -54.00   92.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505    0.0000  240.0000 292

 30 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.8505    0.0000     -     240

 31 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -20.0000     -     240

 32 omega  -46.00   51.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  133.9178 194

 33 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -40.0000     -     240

 34 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   40.0000     -     240

 35 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -60.0000     -     240

 36 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   60.0000     -     240

 37 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.8505    0.0000     -     240

 38 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -20.0000     -     240

 39 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   20.0000     -     240

 40 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -40.0000     -     240

 41 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   40.0000     -     240

 42 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   20.0000     -     240

 43 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   60.0000     -     240

 44 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.8505    0.0000     -     240

 45 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -20.0000     -     240

 46 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   20.0000     -     240

 47 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -40.0000     -     240

 48 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   40.0000     -     240

 49 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -60.0000     -     240

 50 phi    240.00  360.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   60.0000     -     240

 51 omega  -25.00   44.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   19.0000 -180.0000 138

 52 phi    120.00  240.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -60.0000     -     240

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.0018146000
_diffrn_orient_matrix_UB_12      0.0461112000
_diffrn_orient_matrix_UB_13      0.0511959000
_diffrn_orient_matrix_UB_21      0.0666681000
_diffrn_orient_matrix_UB_22      -0.0021681000
_diffrn_orient_matrix_UB_23      0.0283132000
_diffrn_orient_matrix_UB_31      0.0265738000
_diffrn_orient_matrix_UB_32      0.0444019000
_diffrn_orient_matrix_UB_33      -0.0152421000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            161760
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.100
_diffrn_reflns_theta_min         3.315
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       irregular
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.2317
_exptl_crystal_size_mid          0.2162
_exptl_crystal_size_min          0.1815
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0273P)^2^+1.0441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7293
_reflns_number_total             7949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00413c2.cif
_cod_data_source_block           ba_sb17
_cod_database_code               7042699
_audit_block_refno               2227
_audit_block_usercomment         'sb_jb198, irregular, colourless'
_chemical_oxdiff_formula         'C38 H33 N P2'
_chemical_oxdiff_usercomment     'sb_jb198, irregular, colourless'
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.983
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              81586
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            10.66534(12)
_cell_oxdiff_length_b            12.26799(17)
_cell_oxdiff_length_c            13.52930(18)
_cell_oxdiff_angle_alpha         111.4620(12)
_cell_oxdiff_angle_beta          107.2399(11)
_cell_oxdiff_angle_gamma         96.1928(10)
_cell_oxdiff_volume              1526.14(3)
_cell_oxdiff_measurement_reflns_used 42383