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_4086557
_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         'C32 H27 I2 N2 P Zr, C6 D6'
_chemical_formula_sum            'C38 H27 D6 I2 N2 P Zr'
_chemical_formula_weight         899.69
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_block_code                ba_sb28a
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_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
'02.05.2016 15:51:19 CEST UTC+02:00  encif 1.45'
_cell_angle_alpha                90
_cell_angle_beta                 96.7080(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0851(2)
_cell_length_b                   10.29017(12)
_cell_length_c                   21.1915(2)
_cell_measurement_reflns_used    24354
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      30.3280
_cell_measurement_theta_min      3.6120
_cell_volume                     3483.57(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2014 (Giacovazzo et al., 2014)'
_diffrn_ambient_environment      perfluoro
_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 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

--------------------------------------------------------------------------
  1  \w     -9.00  18.00   0.50   15.00    --  -25.00  57.00  90.00   54
  2  \w     27.00  59.00   0.50   15.00    --   26.87 -80.00 135.54   64
  3  \w      2.00  50.00   0.50   15.00    --   26.87  38.00-120.00   96
  4  \w     -4.00  24.00   0.50   15.00    --   26.87  80.00 158.29   56
  5  \w      6.00  84.00   0.50   15.00    --   26.87  57.00-150.00  156
  6  \w     -2.00  25.00   0.50   15.00    --   26.87 -38.00 -60.00   54
  7  \w     60.00  96.00   0.50   15.00    --   26.87  57.00 120.00   72
  8  \w      2.00  43.00   0.50   15.00    --   26.87  77.00 -30.00   82
  9  \w     -1.00  87.00   0.50   15.00    --   26.87  77.00-120.00  176
 10  \w    -44.00  17.00   0.50   15.00    --   26.87 -80.00-140.70  122
 11  \w     34.00  59.00   0.50   15.00    --   26.87 -80.00-140.70   50
 12  \w     -2.00  96.00   0.50   15.00    --   26.87  77.00  60.00  196
 13  \w      1.00  78.00   0.50   15.00    --   26.87  38.00  30.00  154
 14  \w    -40.00  59.00   0.50   15.00    --   26.87 -80.00 -12.19  198
 15  \w     27.00  59.00   0.50   15.00    --   26.87 -80.00  94.65   64
 16  \w    -42.00  57.00   0.50   15.00    --   26.87 -77.00  60.00  198
 17  \w    -42.00  -9.00   0.50   15.00    --   26.87 -77.00-180.00   66
 18  \w     28.00  57.00   0.50   15.00    --   26.87 -77.00-180.00   58
 19  \w    -42.00  59.00   0.50   15.00    --   28.00 -78.00 115.74  202
 20  \w    -29.00  60.00   0.50   15.00    --   28.00 -80.00 -73.53  178
 21  \w    -46.00  -9.00   0.50   15.00    --   26.87 -38.00-120.00   74
 22  \w      6.00  96.00   0.50   15.00    --   26.87  57.00 -60.00  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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0128057000
_diffrn_orient_matrix_UB_12      0.0154833000
_diffrn_orient_matrix_UB_13      -0.0322846000
_diffrn_orient_matrix_UB_21      -0.0237767000
_diffrn_orient_matrix_UB_22      -0.0581488000
_diffrn_orient_matrix_UB_23      -0.0033777000
_diffrn_orient_matrix_UB_31      -0.0352456000
_diffrn_orient_matrix_UB_32      0.0336281000
_diffrn_orient_matrix_UB_33      0.0090487000
_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  0.0705
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            104054
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_min         3.284
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.163
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         10640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+5.6347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8761
_reflns_number_total             10640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00384_si_002.cif
_cod_data_source_block           ba_sb28a
_cod_depositor_comments
'Adding full bibliography for 4086549--4086572.cif.'
_cod_original_cell_volume        3483.58(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4086557
_audit_block_refno               2436
_audit_block_usercomment         'sb365b, irregular, orange'
_chemical_oxdiff_formula         'C38 D6 H27 I2 N2 P1 Zr1'
_chemical_oxdiff_usercomment     'sb365b, irregular, orange'
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.813
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C14(H14A,H14B)
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), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C51(D51), C52(D52), C53(D53), C54(D54), C55(D55), C56(D56)
;
_shelx_res_checksum              94574
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.823
_cell_oxdiff_length_a            16.0845(2)
_cell_oxdiff_length_b            10.28959(16)
_cell_oxdiff_length_c            21.1936(4)
_cell_oxdiff_angle_alpha         90.0226(13)
_cell_oxdiff_angle_beta          96.7091(14)
_cell_oxdiff_angle_gamma         89.9801(13)
_cell_oxdiff_volume              3483.58(10)
_cell_oxdiff_measurement_reflns_used 24354