Utilising an anilido-imino ligand to stabilise zinc-phosphanide complexes: reactivity and fluorescent properties.
Webb, Dylan; Fulton, J. Robin; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8094–8105; doi:10.1039/c9dt00681h

data_7049731
_publ_section_title
;
 Utilising an anilido-imino ligand to stabilise zinc-phosphanide
 complexes: reactivity and fluorescent properties.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8094
_journal_page_last               8105
_journal_paper_doi               10.1039/c9dt00681h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C64 H82 N4 Te Zn2, C3 H7'
_chemical_formula_sum            'C67 H89 N4 Te Zn2'
_chemical_formula_weight         1208.76
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-09
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;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                85.696(3)
_cell_angle_beta                 78.852(4)
_cell_angle_gamma                63.031(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1052(5)
_cell_length_b                   12.8767(5)
_cell_length_c                   22.5863(11)
_cell_measurement_reflns_used    11000
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      71.5560
_cell_measurement_theta_min      4.9360
_cell_volume                     3078.2(3)
_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
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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)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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;
  1 omega   20.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega   40.00   98.00   1.0000   10.0000
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  3 omega   63.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega   55.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega   65.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   49.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   59.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega   42.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega   52.00  104.00   1.0000   10.0000
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 10 omega   38.00   74.00   1.0000   10.0000
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 11 omega   43.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 26

 12 omega   97.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 37

 13 omega  146.00  176.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 30

 14 omega  145.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 33

 15 omega  104.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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 16 omega   94.00  133.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 39

 17 omega   90.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  120.0000 77

 18 omega   45.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 27

 19 omega   45.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 37

 20 omega   41.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 51

 21 omega   40.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 50

 22 omega   38.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 26

 23 omega    9.00   49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000   60.0000 40

 24 omega    6.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -19.0000    0.0000 59

 25 omega   17.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104   38.0000  -60.0000 76

 26 omega    9.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104   77.0000  -60.0000 92

 27 omega   10.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104   77.0000 -180.0000 47

 28 omega  -34.00   -5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -19.0000    0.0000 29

 29 omega  -27.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000  120.0000 49

 30 omega   11.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000  150.0000 35

 31 omega   36.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104 -125.0000   90.0000 53

 32 omega  -24.00    8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000  150.0000 32

 33 omega    4.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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 34 omega  -30.00    0.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000 -180.0000 30
;
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_diffrn_measurement_method       '\w scans'
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_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_number            22600
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
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_diffrn_reflns_theta_max         72.120
_diffrn_reflns_theta_min         4.165
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
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_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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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)
Numerical absorption correction based on gaussian integration over
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Empirical absorption correction using spherical harmonics,
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;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1262
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0389
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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^)+(0.0325P)^2^+5.6266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10715
_reflns_number_total             11772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00681h2.cif
_cod_data_source_block           Compound-10
_cod_depositor_comments
'Adding full bibliography for 7049727--7049732.cif.'
_cod_original_cell_volume        3078.3(3)
_cod_database_code               7049731
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C44 H51 N2 P Zn Te2'
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.483
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C18(H18), C47(H47), C30(H30), C50(H50), C62(H62), C59(H59), C27(H27), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B), C67(H67A,H67B)
2.c Aromatic/amide H refined with riding coordinates:
 C43(H43), C40(H40), C45(H45), C5(H5), C44(H44), C37(H37), C39(H39), C55(H55),
 C8(H8), C25(H25), C38(H38), C57(H57), C56(H56), C11(H11), C23(H23), C12(H12),
 C24(H24), C7(H7), C13(H13), C6(H6)
2.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C4(H4A,H4B,H4C), C63(H63A,H63B,H63C), C31(H31A,H31B,
 H31C), C48(H48A,H48B,H48C), C32(H32A,H32B,H32C), C64(H64A,H64B,H64C), C19(H19A,
 H19B,H19C), C52(H52A,H52B,H52C), C61(H61A,H61B,H61C), C49(H49A,H49B,H49C),
 C20(H20A,H20B,H20C), C60(H60A,H60B,H60C), C51(H51A,H51B,H51C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C65(H65A,H65B,H65C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'