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_7049728
_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         'C44 H63 N2 P Te2 Zn'
_chemical_formula_sum            'C44 H63 N2 P Te2 Zn'
_chemical_formula_weight         971.50
_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_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     dual
_audit_creation_date             2019-02-07
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Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2019-02-14 deposited with the CCDC.    2019-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.60(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.374(3)
_cell_length_b                   10.6381(15)
_cell_length_c                   24.802(4)
_cell_measurement_reflns_used    10063
_cell_measurement_temperature    290.45(17)
_cell_measurement_theta_max      71.6680
_cell_measurement_theta_min      4.1320
_cell_volume                     4719.2(14)
_computing_cell_refinement
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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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_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)
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_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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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.45(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
  1 omega   20.00   65.00   1.0000    1.0600
omega____ theta____ kappa____ phi______ frames
    -       36.0104   38.0000  120.0000 45

  2 omega   40.00   94.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 54

  3 omega   72.00  109.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 37

  4 omega   51.00   77.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 26

  5 omega   40.00   87.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 47

  6 omega   45.00  108.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -60.0000 63

  7 omega   47.00   72.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 25

  8 omega   46.00   71.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 25

  9 omega   42.00   75.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 33

 10 omega   90.00  178.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   90.0000 88

 11 omega   93.00  176.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 83

 12 omega   60.00   88.00   1.0000    1.0600
omega____ theta____ kappa____ phi______ frames
    -       36.0104 -125.0000 -180.0000 28

 13 omega   41.00  116.00   1.0000    4.2500
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 75

 14 omega   20.00   51.00   1.0000    1.0600
omega____ theta____ kappa____ phi______ frames
    -       36.0104 -100.0000   86.0000 31

 15 omega    9.00   75.00   1.0000    1.0600
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -99.0000  -30.0000 66

 16 omega   -6.00   65.00   1.0000    1.0600
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -19.0000 -150.0000 71

 17 omega  -29.00   63.00   1.0000    1.0600
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -77.0000 -150.0000 92

 18 omega  -13.00   46.00   1.0000    1.0600
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000   90.0000 59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0289363000
_diffrn_orient_matrix_UB_12      -0.0986398000
_diffrn_orient_matrix_UB_13      0.0490973000
_diffrn_orient_matrix_UB_21      0.0208622000
_diffrn_orient_matrix_UB_22      -0.0876151000
_diffrn_orient_matrix_UB_23      -0.0408717000
_diffrn_orient_matrix_UB_31      0.0783459000
_diffrn_orient_matrix_UB_32      0.0597725000
_diffrn_orient_matrix_UB_33      0.0209460000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19454
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.931
_diffrn_reflns_theta_min         4.583
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63036
_exptl_absorpt_correction_type   multi-scan
_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.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.2672
_exptl_crystal_size_mid          0.1753
_exptl_crystal_size_min          0.0967
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+3.8644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7838
_reflns_number_total             9004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00681h2.cif
_cod_data_source_block           Compound-8
_cod_depositor_comments
'Adding full bibliography for 7049727--7049732.cif.'
_cod_original_cell_volume        4719.1(14)
_cod_database_code               7049728
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C44 H63 N2 P Te2 Zn'
_shelx_estimated_absorpt_t_max   0.421
_shelx_estimated_absorpt_t_min   0.160
_reflns_odcompleteness_completeness 99.60
_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:
 C15(H15), C18(H18), C33(H33), C27(H27), C39(H39), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C34(H34A,H34B), C43(H43A,H43B), C38(H38A,H38B), C42(H42A,
 H42B), C40(H40A,H40B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C11(H11), C6(H6), C13(H13), C7(H7), C12(H12), C25(H25),
 C23(H23), C24(H24)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C17(H17A,H17B,H17C), C28(H28A,
 H28B,H28C), C32(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'