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_7049730
_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 H51 N2 P Zn'
_chemical_formula_sum            'C44 H51 N2 P Zn'
_chemical_formula_weight         704.20
_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             2019-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                97.589(2)
_cell_angle_beta                 104.345(2)
_cell_angle_gamma                98.248(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9460(3)
_cell_length_b                   13.4527(3)
_cell_length_c                   13.6087(4)
_cell_measurement_reflns_used    8723
_cell_measurement_temperature    291.24(10)
_cell_measurement_theta_max      71.7240
_cell_measurement_theta_min      4.2230
_cell_volume                     1891.78(9)
_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
;
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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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
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_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega   23.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega   71.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104   38.0000    0.0000 32

  3 omega   36.00   99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104   77.0000 -120.0000 63

  4 omega  108.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -30.0000 47

  5 omega  100.00  175.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 75

  6 omega   84.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 25

  7 omega   64.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 52

  8 omega   50.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 27

  9 omega   43.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 45

 10 omega   55.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 26

 11 omega   45.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 63

 12 omega   55.00   92.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 37

 13 omega   48.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 56

 14 omega   56.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 51

 15 omega   44.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 38

 16 omega   41.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 57

 17 omega   38.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 35

 18 omega   45.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 28

 19 omega   38.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 20 omega   71.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -30.0000 107

 21 omega   43.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 46

 22 omega   26.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104 -125.0000  -60.0000 63

 23 omega   18.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -38.0000  -30.0000 27

 24 omega    1.00   60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -99.0000   30.0000 59

 25 omega   23.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104 -125.0000   90.0000 40

 26 omega   34.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -99.0000  120.0000 41

 27 omega  -13.00   25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000   30.0000 38

 28 omega  -30.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000  150.0000 51

 29 omega  -33.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -38.0000   60.0000 77

 30 omega   13.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0104   77.0000 -180.0000 90
;
_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      -0.1067640000
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_diffrn_orient_matrix_UB_21      0.1016732000
_diffrn_orient_matrix_UB_22      0.0751785000
_diffrn_orient_matrix_UB_23      0.0871102000
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_diffrn_orient_matrix_UB_32      0.0837770000
_diffrn_orient_matrix_UB_33      -0.0670814000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12976
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.705
_diffrn_reflns_theta_min         4.354
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.533
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   gaussian
_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)
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            'light yellow'
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       prism
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.1862
_exptl_crystal_size_mid          0.1787
_exptl_crystal_size_min          0.1364
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.290
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     442
_refine_ls_number_reflns         7215
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0376P)^2^+0.9329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6711
_reflns_number_total             7215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00681h2.cif
_cod_data_source_block           Compound-5
_cod_depositor_comments
'Adding full bibliography for 7049727--7049732.cif.'
_cod_database_code               7049730
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C44 H51 N2 P Zn'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C23 \\sim C24: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4.a Ternary CH refined with riding coordinates:
 C30(H30), C27(H27), C18(H18), C15(H15)
4.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C23(H23), C34(H34), C41(H41), C24(H24), C8(H8), C35(H35), C44(H44),
 C5(H5), C13(H13), C25(H25), C7(H7), C38(H38), C42(H42), C12(H12), C6(H6),
 C43(H43), C11(H11), C37(H37), C36(H36)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C19(H19A,H19B,
 H19C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C20(H20A,
 H20B,H20C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'