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_4344802
_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         'C49 H54 Cl2 N P3 Zr'
_chemical_formula_sum            'C49 H54 Cl2 N P3 Zr'
_chemical_formula_weight         911.96
_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   mixed
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'Thu Mar 12 15:15:47 2015'
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Olex2 1.2
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;
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'12.03.2015 16:35:53 CET UTC+01:00  encif 1.29'
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_cell_measurement_reflns_used    41185
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.5400
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
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;
  1 omega  -38.00  -12.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega    2.00   39.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega   18.00   57.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega  -44.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -80.0000   81.5787 206

  5 omega  -44.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -80.0000    1.6379 206

  6 omega   -8.00   19.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -57.0000    0.0000 54

  7 omega   10.00   83.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000  -60.0000 146

  8 omega    2.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   38.0000   60.0000 114

  9 omega   68.00   99.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   38.0000   60.0000 62

 10 omega   -2.00   24.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000  -90.0000 52

 11 omega   -2.00   71.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000   90.0000 146

 12 omega   -1.00   97.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000 -180.0000 196

 13 omega   -3.00   38.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000    0.0000 82

 14 omega   32.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000  -61.9149 54

 15 omega  -41.00    5.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000  -61.9149 92

 16 omega  -43.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -79.0000  149.0775 204

 17 omega   34.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000  103.1456 50

 18 omega  -42.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000 -139.4439 202

 19 omega  -42.00   48.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -57.0000 -150.0000 180

 20 omega   -3.00   97.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000  -60.0000 200

 21 omega  -43.00   57.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -77.0000   30.0000 200

 22 omega    6.00   96.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000   90.0000 180

 23 omega  -42.00   48.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -57.0000  150.0000 180

 24 omega  -42.00   48.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -57.0000  -60.0000 180

 25 omega    6.00   96.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000 -120.0000 180

 26 omega    6.00   31.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000   60.0000 50

 27 omega   -3.00   97.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000  150.0000 200

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_11      0.0560839000
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_diffrn_orient_matrix_UB_21      -0.0058764000
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_diffrn_orient_matrix_UB_33      0.0155814000
_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  0.0461
_diffrn_reflns_av_unetI/netI     0.0339
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_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            121150
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         3.233
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.431
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
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            red
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_exptl_crystal_size_mid          0.168
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_refine_diff_density_max         1.437
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         18230
_refine_ls_number_restraints     0
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+1.5817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15246
_reflns_number_total             18230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02498_si_002.cif
_cod_data_source_block           ga_gp28_sq
_cod_database_code               4344802
_audit_block_refno               2373
_audit_block_usercomment         'gp750, irregular, red'
_chemical_oxdiff_formula         'C50 H57 Cl2 N P4 Zr'
_chemical_oxdiff_usercomment     'gp750, irregular, red'
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.958
_reflns_odcompleteness_completeness 99.80
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C9(H9), C11(H11), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
  C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              34064
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.87889(17)
_cell_oxdiff_length_b            14.18501(18)
_cell_oxdiff_length_c            16.2618(2)
_cell_oxdiff_angle_alpha         66.3864(12)
_cell_oxdiff_angle_beta          85.4794(11)
_cell_oxdiff_angle_gamma         75.2037(11)
_cell_oxdiff_volume              2630.88(6)
_cell_oxdiff_measurement_reflns_used 41185
_platon_squeeze_void_probe_radius 1.20