Closely Related Benzylene-Linked Diamidophosphine Scaffolds and Their Zirconium and Hafnium Complexes: How Small Changes of the Ligand Result in Different Complex Stabilities and Reactivities
Batke, Sonja; Sietzen, Malte; Merz, Lukas; Wadepohl, Hubert; Ballmann, Joachim; Organometallics 35 (2016) 2294–; doi:10.1021/acs.organomet.6b00384

data_4086551
_publ_section_title
;
 Closely Related Benzylene-Linked Diamidophosphine Scaffolds and Their
 Zirconium and Hafnium Complexes: How Small Changes of the Ligand Result
 in Different Complex Stabilities and Reactivities
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2294
_journal_paper_doi               10.1021/acs.organomet.6b00384
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C40 H47 N4 P Zr, C2.5 H6'
_chemical_formula_sum            'C42.5 H53 N4 P Zr'
_chemical_formula_weight         742.08
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
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'Tue Apr 28 14:25:39 2015'
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Olex2 1.2
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'28.04.2015 14:28:31 CEST UTC+02:00  encif 1.29'
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_cell_formula_units_Z            8
_cell_length_a                   18.9485(3)
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_cell_measurement_reflns_used    28684
_cell_measurement_temperature    120(1)
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
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_diffrn_measurement_details
;
  1 omega   -3.00   23.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000  120.0000 52

  2 omega  -41.00   32.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -57.0000   30.0000 146

  3 omega    7.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000 -180.0000 86

  4 omega   12.00   62.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000  -60.0000 100

  5 omega   -1.00   46.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   19.0000   60.0000 94

  6 omega   -3.00   94.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000 -120.0000 194

  7 omega   10.00   96.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000 -180.0000 172

  8 omega   -2.00   24.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   78.0000   55.9698 52

  9 omega    1.00   99.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000   90.0000 196

 10 omega   -5.00   20.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   80.0000   28.0361 50

 11 omega  -42.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -79.0000  -11.2935 202

 12 omega  -38.00   58.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -79.0000 -134.5197 192

 13 omega  -25.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -79.0000  -70.6415 168

 14 omega  -43.00   60.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000  134.0474 206

 15 omega   34.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000   36.5990 50

 16 omega  -46.00   52.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -38.0000  120.0000 196

 17 omega  -46.00  -21.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -38.0000 -120.0000 50

 18 omega    6.00   96.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000 -150.0000 180

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.0043862000
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_diffrn_orient_matrix_UB_21      -0.0195350000
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_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            114232
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         3.271
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.365
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_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
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            'light yellow'
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       irregular
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_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         13469
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_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0681
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+11.0624P] where P=(Fo^2^+2Fc^2^)/3'
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_cod_depositor_comments
'Adding full bibliography for 4086549--4086572.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C42.50 H53 N4 P Zr'
_cod_database_code               4086551
_audit_block_refno               2422
_audit_block_usercomment         'MS357, irregular, light yellow'
_chemical_oxdiff_formula         'C42.5 H53 N4 P1 Zr1'
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H53A(0.5) H53B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C52(H52A,H52B), C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C26(H26),
  C30(H30), C32(H32), C34(H34)
3.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              36888
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            18.9490(2)
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_cell_oxdiff_length_c            30.4111(4)
_cell_oxdiff_angle_alpha         89.9873(11)
_cell_oxdiff_angle_beta          105.8735(12)
_cell_oxdiff_angle_gamma         89.9651(11)
_cell_oxdiff_volume              7631.48(18)
_cell_oxdiff_measurement_reflns_used 28683