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_4086567
_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         'C46 H41 Hf N2 P'
_chemical_formula_sum            'C46 H41 Hf N2 P'
_chemical_formula_weight         831.27
_chemical_properties_physical    'air-sensitive, moisture-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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_sb35
_audit_creation_date             2015-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
'30.10.2015 13:48:14 CET UTC+01:00  encif 1.36'
_cell_angle_alpha                100.832(2)
_cell_angle_beta                 92.9449(19)
_cell_angle_gamma                101.4852(17)
_cell_formula_units_Z            2
_cell_length_a                   9.69030(19)
_cell_length_b                   13.2661(3)
_cell_length_c                   15.1478(4)
_cell_measurement_reflns_used    17739
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.5880
_cell_measurement_theta_min      3.6370
_cell_volume                     1866.30(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'SUPERFLIP (Palatinus, 2007-2009)'
_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 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

--------------------------------------------------------------------------
  1  \w      2.00  84.00   0.50   20.00    --   19.75  57.00 120.00  164
  2  \w    -45.00  38.00   0.50   20.00    --   19.75 -38.00  30.00  166
  3  \w    -20.00  63.00   0.50   20.00    --   19.75 -99.00 -30.00  166
  4  \w      2.00  85.00   0.50   20.00    --   19.75  57.00-150.00  166
  5  \w    -20.00  63.00   0.50   20.00    --   19.75 -99.00-180.00  166
  6  \w     -2.00  80.00   0.50   20.00    --   19.75  77.00 -30.00  164
  7  \w    -12.00  91.00   0.50   20.00    --   19.75  77.00-150.00  206
  8  \w     -2.00  89.00   0.50   20.00    --   19.75  57.00 -30.00  182
  9  \w    -20.00  63.00   0.50   20.00    --   19.75 -99.00   0.00  166
 10  \w     -2.00  89.00   0.50   20.00    --   19.75  57.00  90.00  182
 11  \w    -51.00  51.00   0.50   20.00    --   19.75 -77.00-150.00  204
 12  \w    -20.00  63.00   0.50   20.00    --   19.75 -99.00 120.00  166
 13  \w     -2.00  85.00   0.50   20.00    --   19.75  57.00   0.00  174
 14  \w    -49.00  41.00   0.50   20.00    --   19.75 -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      0.0051548000
_diffrn_orient_matrix_UB_12      0.0151637000
_diffrn_orient_matrix_UB_13      -0.0423896000
_diffrn_orient_matrix_UB_21      -0.0735644000
_diffrn_orient_matrix_UB_22      -0.0010232000
_diffrn_orient_matrix_UB_23      -0.0033667000
_diffrn_orient_matrix_UB_31      0.0137324000
_diffrn_orient_matrix_UB_32      0.0536005000
_diffrn_orient_matrix_UB_33      0.0220043000
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            41675
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.334
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.872
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            'light yellow'
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.657
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0390P)^2^+4.3388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6883
_reflns_number_total             7614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00384_si_002.cif
_cod_data_source_block           ba_sb35
_cod_depositor_comments
'Adding full bibliography for 4086549--4086572.cif.'
_cod_original_cell_volume        1866.30(7)
_cod_database_code               4086567
_audit_block_refno               2543
_audit_block_usercomment         'sb399, light yellow, block'
_chemical_oxdiff_formula         'C46 H41 Hf N2 P'
_chemical_oxdiff_usercomment     'sb399, light yellow, block'
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.762
_reflns_odcompleteness_completeness 99.79
_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), C33(H33A,H33B), C40(H40A,H40B)
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),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46)
;
_shelx_res_checksum              74201
_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 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.897
_cell_oxdiff_length_a            9.69030(19)
_cell_oxdiff_length_b            13.2661(3)
_cell_oxdiff_length_c            15.1478(4)
_cell_oxdiff_angle_alpha         100.832(2)
_cell_oxdiff_angle_beta          92.9449(19)
_cell_oxdiff_angle_gamma         101.4852(17)
_cell_oxdiff_volume              1866.30(7)
_cell_oxdiff_measurement_reflns_used 17739