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_4086555
_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 Ti'
_chemical_formula_sum            'C32 H27 I2 N2 P Ti'
_chemical_formula_weight         772.22
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_sb54
_audit_creation_date             2016-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
'23.03.2016 17:20:16 CET UTC+01:00  encif 1.40'
_cell_angle_alpha                90
_cell_angle_beta                 102.2165(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.75732(8)
_cell_length_b                   14.56140(10)
_cell_length_c                   17.37463(12)
_cell_measurement_reflns_used    44819
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.2200
_cell_measurement_theta_min      3.3010
_cell_volume                     2907.23(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (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 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

--------------------------------------------------------------------------
  1  \w      7.00  96.00   0.50   15.00    --   27.02  57.00 120.00  178
  2  \w    -42.00  48.00   0.50   15.00    --   27.02 -57.00  60.00  180
  3  \w      2.00  99.00   0.50   15.00    --   27.02  38.00  30.00  194
  4  \w      7.00  96.00   0.50   15.00    --   27.02  57.00-150.00  178
  5  \w    -20.00  69.00   0.50   15.00    --   27.02 -99.00 -90.00  178
  6  \w    -42.00  48.00   0.50   15.00    --   27.02 -57.00 -30.00  180
  7  \w    -20.00  69.00   0.50   15.00    --   27.02 -99.00-180.00  178
  8  \w     -3.00  75.00   0.50   15.00    --   27.02  77.00  30.00  156
  9  \w     -3.00  42.00   0.50   15.00    --   27.02  77.00-180.00   90
 10  \w      3.00  36.00   0.50   15.00    --   27.02  77.00 -60.00   66
 11  \w    -45.00  52.00   0.50   15.00    --   27.02 -38.00-150.00  194
 12  \w     -3.00  85.00   0.50   15.00    --   27.02  77.00  60.00  176
 13  \w     38.00  67.00   0.50   15.00    --   27.02 -99.00  30.00   58
 14  \w     14.00  90.00   0.50   15.00    --   27.02  77.00-150.00  152
 15  \w      8.00  91.00   0.50   15.00    --   27.02  38.00 -30.00  166
 16  \w      7.00  32.00   0.50   15.00    --   27.02  57.00-180.00   50
 17  \w      2.00  28.00   0.50   15.00    --   27.02  38.00-180.00   52
;
_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      0.0077882000
_diffrn_orient_matrix_UB_12      -0.0435428000
_diffrn_orient_matrix_UB_13      -0.0164378000
_diffrn_orient_matrix_UB_21      -0.0103281000
_diffrn_orient_matrix_UB_22      0.0198797000
_diffrn_orient_matrix_UB_23      -0.0381162000
_diffrn_orient_matrix_UB_31      0.0603532000
_diffrn_orient_matrix_UB_32      0.0090448000
_diffrn_orient_matrix_UB_33      0.0046218000
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            87824
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.364
_diffrn_reflns_theta_min         3.009
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.498
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41p (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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         10053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+2.5687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9262
_reflns_number_total             10053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00384_si_002.cif
_cod_data_source_block           ba_sb54
_cod_depositor_comments
'Adding full bibliography for 4086549--4086572.cif.'
_cod_original_cell_volume        2907.23(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4086555
_audit_block_refno               2685
_audit_block_usercomment         'sb442, irregular, black'
_chemical_oxdiff_formula         'C32 H27 I2 Ti P N2'
_chemical_oxdiff_usercomment     'sb442, irregular, black'
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.788
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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)
;
_shelx_res_checksum              52257
_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 1.086
_oxdiff_exptl_absorpt_empirical_full_min 0.888
_cell_oxdiff_length_a            11.75684(9)
_cell_oxdiff_length_b            14.56072(12)
_cell_oxdiff_length_c            17.37480(19)
_cell_oxdiff_angle_alpha         89.9887(8)
_cell_oxdiff_angle_beta          102.1955(8)
_cell_oxdiff_angle_gamma         90.0293(7)
_cell_oxdiff_volume              2907.23(5)
_cell_oxdiff_measurement_reflns_used 44819