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_4344795
_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         'C41 H60 Cl N P2 Ti, C4 H10 O'
_chemical_formula_sum            'C45 H70 Cl N O P2 Ti'
_chemical_formula_weight         786.31
_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   mixed
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'Mon Oct 12 14:35:06 2015'
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Olex2 1.2
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'12.10.2015 14:41:19 CEST UTC+02:00  encif 1.35'
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_cell_measurement_reflns_used    13535
_cell_measurement_temperature    120(1)
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
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_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
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_diffrn_measurement_details
;
  1 omega    0.00   81.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   64.0000 -172.0000 162

  2 omega  -46.00   36.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -38.0000  120.0000 164

  3 omega    1.00   84.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   57.0000  -60.0000 166

  4 omega  -20.00   61.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -99.0000   30.0000 162

  5 omega  -20.00   61.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -99.0000  -90.0000 162

  6 omega   -2.00   81.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   77.0000   60.0000 166

  7 omega  -54.00   44.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -38.0000   30.0000 196

  8 omega   -3.00   88.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   57.0000    0.0000 182

  9 omega  -50.00   40.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -57.0000  -30.0000 180

 10 omega  -20.00   61.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -99.0000 -180.0000 162

 11 phi    120.00  240.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
  18.7723   18.7723  -20.0000     -     240

 12 omega   -3.00   15.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   57.0000  120.0000 36

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
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_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0157284000
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_diffrn_orient_matrix_UB_21      0.0412040000
_diffrn_orient_matrix_UB_22      0.0209627000
_diffrn_orient_matrix_UB_23      0.0182495000
_diffrn_orient_matrix_UB_31      0.0379144000
_diffrn_orient_matrix_UB_32      -0.0043617000
_diffrn_orient_matrix_UB_33      -0.0188473000
_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  0.0852
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            73616
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         3.247
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.357
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_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.174
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_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.069
_refine_diff_density_max         2.025
_refine_diff_density_min         -0.646
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0741
_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^)+(0.1142P)^2^+6.4822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6192
_reflns_number_total             7927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02498_si_002.cif
_cod_data_source_block           ga_gp43
_cod_original_cell_volume        4450.39(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4344795
_audit_block_refno               2552
_audit_block_usercomment         'gp916, irregualr, red'
_chemical_oxdiff_formula         'C45 H70 Cl1 N1 O1 P2 Ti1'
_chemical_oxdiff_usercomment     'gp916, irregualr, red'
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.965
_reflns_odcompleteness_completeness 97.20
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_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:
 C24(H24), C27(H27), C30(H30), C33(H33)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C51(H51A,H51B), C53(H53A,H53B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C9(H9), C11(H11), C38(H38), C39(H39), C40(H40), C41(H41),
 C42(H42)
2.d Idealised Me refined as rotating group:
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 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
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 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C52(H52A,H52B,
 H52C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              27649
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.2894(2)
_cell_oxdiff_length_b            14.4303(3)
_cell_oxdiff_length_c            25.2884(5)
_cell_oxdiff_angle_alpha         89.9711(17)
_cell_oxdiff_angle_beta          97.0858(17)
_cell_oxdiff_angle_gamma         90.0527(17)
_cell_oxdiff_volume              4450.39(16)
_cell_oxdiff_measurement_reflns_used 13535