Synthesis and Reactivity of Group 4 Metal Benzyl Complexes Supported by Carbazolide-Based PNP Pincer Ligands.
Plundrich, Gudrun T.; Wadepohl, Hubert; Gade, Lutz H.; Inorganic chemistry 55 (2015) 353–; doi:10.1021/acs.inorgchem.5b02498

data_4344790
_publ_section_title
;
 Synthesis and Reactivity of Group 4 Metal Benzyl Complexes Supported by
 Carbazolide-Based PNP Pincer Ligands.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              353
_journal_paper_doi               10.1021/acs.inorgchem.5b02498
_journal_volume                  55
_journal_year                    2015
_chemical_formula_moiety         'C34 H54 Cl3 Hf N P2'
_chemical_formula_sum            'C34 H54 Cl3 Hf N P2'
_chemical_formula_weight         823.56
_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     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_gp37
_audit_creation_date             2015-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
'23.10.2015 15:50:24 CEST UTC+02:00  encif 1.36'
_cell_angle_alpha                90
_cell_angle_beta                 110.629(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.084(11)
_cell_length_b                   11.776(6)
_cell_length_c                   26.438(11)
_cell_measurement_reflns_used    7379
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.73
_cell_measurement_theta_min      2.22
_cell_volume                     7309(6)
_computing_cell_refinement
;
SAINT (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction
'SAINT V8.34A (Bruker AXS, 1997-2013),SADABS-2014_5 (Sheldrick and Bruker AXS, 1997-2014)'
_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 polyether oil / N~2~'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            187453
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.540
_diffrn_reflns_theta_min         1.935
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.185
_exptl_absorpt_correction_T_max  0.4950
_exptl_absorpt_correction_T_min  0.3998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.570
_refine_diff_density_min         -1.660
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         25432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0220P)^2^+15.0567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20357
_reflns_number_total             25432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02498_si_002.cif
_cod_data_source_block           ga_gp37
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4344790
_audit_block_refno               2455
_audit_block_usercomment         gp-11-32
_shelx_estimated_absorpt_t_max   0.568
_shelx_estimated_absorpt_t_min   0.568
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C74(H74), C77(H77), C80(H80), C83(H83), C30(H30), C24(H24), C27(H27), C33(H33)
2.b Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C65(H65A,H65B), C14(H14A,H14B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C54(H54), C56(H56), C59(H59), C61(H61), C4(H4), C6(H6), C9(H9), C11(H11)
2.d Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C76(H76A,
 H76B,H76C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C),
 C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C26(H26A,H26B,
 H26C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C34(H34A,H34B,H34C), C28(H28A,
 H28B,H28C), C32(H32A,H32B,H32C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C),
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              83011
_olex2_submission_special_instructions 'No special instructions were received'