Diamidophosphines with six-membered chelates and their coordination chemistry with group 4 metals: development of a trimethylene-methane-tethered [PN2]-type "molecular claw".
Batke, S.; Kothe, T.; Haas, M.; Wadepohl, H.; Ballmann, J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 3528–3540; doi:10.1039/c5dt04911c

data_7038123
_publ_section_title
;
 Diamidophosphines with six-membered chelates and their coordination
 chemistry with group 4 metals: development of a
 trimethylene-methane-tethered [PN2]-type &quot;molecular claw&quot;.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3528
_journal_page_last               3540
_journal_paper_doi               10.1039/c5dt04911c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C24 H27 Cl2 Hf N2 P, C H2 Cl2'
_chemical_formula_sum            'C25 H29 Cl4 Hf N2 P'
_chemical_formula_weight         708.76
_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_tk10
_audit_creation_date
;
'Mon Jul 06 15:49:16 2015'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                66.6471(16)
_cell_angle_beta                 84.8482(13)
_cell_angle_gamma                75.6062(13)
_cell_formula_units_Z            2
_cell_length_a                   8.58828(12)
_cell_length_b                   11.7688(2)
_cell_length_c                   14.5396(3)
_cell_measurement_reflns_used    25862
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.1220
_cell_measurement_theta_min      3.8900
_cell_volume                     1306.77(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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 0.954
_diffrn_measurement_details
;
  1 omega   -8.00   77.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224 -113.0000  152.0000 170

  2 omega   -3.00   56.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   77.0000 -120.0000 118

  3 omega  -38.00   38.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -57.0000  -30.0000 152

  4 omega   47.00   74.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  178.0000  -30.0000 54

  5 omega   35.00  102.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  178.0000  150.0000 134

  6 omega    3.00   38.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   77.0000   60.0000 70

  7 omega  -21.00   28.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -19.0000   90.0000 98

  8 omega   -3.00   90.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   77.0000  -30.0000 186

  9 omega   -2.00   53.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   77.0000  120.0000 110

 10 omega    2.00   99.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   38.0000  -60.0000 194

 11 omega  -43.00   53.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -77.0000 -150.0000 192

 12 omega  -12.00   69.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -99.0000  -30.0000 162

 13 omega    7.00   89.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   57.0000 -150.0000 164

 14 omega  -13.00  100.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   19.0000  150.0000 226

 15 omega    7.00   96.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   57.0000  -60.0000 178

 16 omega   34.00  104.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224 -178.0000    0.0000 140

 17 omega    7.00   96.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   57.0000   30.0000 178

 18 omega  -45.00   35.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224  -38.0000    0.0000 160

 19 omega    2.00   99.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       27.0224   38.0000  150.0000 194

;
_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      0.0301420000
_diffrn_orient_matrix_UB_12      -0.0224946000
_diffrn_orient_matrix_UB_13      0.0494835000
_diffrn_orient_matrix_UB_21      -0.0786408000
_diffrn_orient_matrix_UB_22      0.0187474000
_diffrn_orient_matrix_UB_23      0.0167489000
_diffrn_orient_matrix_UB_31      -0.0133430000
_diffrn_orient_matrix_UB_32      -0.0608221000
_diffrn_orient_matrix_UB_33      0.0097307000
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.435
_diffrn_reflns_theta_min         3.454
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    4.479
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
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    1.801
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.143
_refine_diff_density_max         0.929
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         8967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0326P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8388
_reflns_number_total             8967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04911c2.cif
_cod_data_source_block           ba_tk10
_cod_depositor_comments
'Adding full bibliography for 7038121--7038129.cif.'
_cod_database_code               7038123
_audit_block_refno               2476
_audit_block_usercomment         'NPNHfCl2 colourless block'
_chemical_oxdiff_formula         'C25 h29 Cl4 Hf1 N2 P1'
_chemical_oxdiff_usercomment     'NPNHfCl2 colourless block'
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.663
_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), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              77051
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            8.58828(12)
_cell_oxdiff_length_b            11.7688(2)
_cell_oxdiff_length_c            14.5396(2)
_cell_oxdiff_angle_alpha         66.6471(16)
_cell_oxdiff_angle_beta          84.8482(13)
_cell_oxdiff_angle_gamma         75.6062(13)
_cell_oxdiff_volume              1306.77(4)
_cell_oxdiff_measurement_reflns_used 25862