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_7049729
_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 Se2 Zn'
_chemical_formula_sum            'C44 H63 N2 P Se2 Zn'
_chemical_formula_weight         874.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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)
;
_audit_update_record
;
2019-02-14 deposited with the CCDC.    2019-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.7020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0660(2)
_cell_length_b                   10.35150(10)
_cell_length_c                   24.6114(3)
_cell_measurement_reflns_used    21327
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      71.7010
_cell_measurement_theta_min      4.6390
_cell_volume                     4481.02(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
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   66.00  103.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104   57.0000  -30.0000 37

  2 omega   56.00  102.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104   38.0000 -120.0000 46

  3 omega   37.00   93.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104   57.0000 -180.0000 56

  4 omega   38.00   91.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 53

  5 omega   51.00   86.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 35

  6 omega   84.00  133.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -86.0000 -129.0000 49

  7 omega   94.00  145.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000    0.0000 51

  8 omega  132.00  176.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 44

  9 omega   59.00  104.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 45

 10 omega   79.00  116.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 37

 11 omega   55.00   99.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  150.0000 44

 12 omega   41.00   96.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 55

 13 omega   42.00   68.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000    0.0000 26

 14 omega   41.00   93.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 52

 15 omega   47.00  114.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 67

 16 omega   46.00   71.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -99.0000  -60.0000 25

 17 omega   62.00   89.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104 -125.0000  -90.0000 27

 18 omega   42.00  108.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -150.0000 66

 19 omega   53.00   80.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -86.0000 -129.0000 27

 20 omega   41.00   83.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 42

 21 omega   39.00  173.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000  -60.0000 134

 22 omega   42.00   94.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 52

 23 omega   38.00   88.00   1.0000   15.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 50

 24 omega   24.00   87.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104 -125.0000  150.0000 63

 25 omega   -2.00   24.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000    0.0000 26

 26 omega   15.00   41.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -99.0000  -60.0000 26

 27 omega    6.00   35.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -99.0000  -90.0000 29

 28 omega  -18.00   43.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000  -90.0000 61

 29 omega  -30.00   -5.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -57.0000    0.0000 25

 30 omega  -32.00   52.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -38.0000   60.0000 84

 31 omega   24.00   50.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104   57.0000  120.0000 26

 32 omega   13.00   97.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104   77.0000   30.0000 84

 33 omega   31.00   56.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104   57.0000  -30.0000 25

 34 omega  -31.00   53.00   1.0000    3.8500
omega____ theta____ kappa____ phi______ frames
    -       36.0104  -77.0000 -150.0000 84
;
_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      -0.0452315000
_diffrn_orient_matrix_UB_12      -0.0853520000
_diffrn_orient_matrix_UB_13      -0.0533488000
_diffrn_orient_matrix_UB_21      -0.0007127000
_diffrn_orient_matrix_UB_22      0.1110319000
_diffrn_orient_matrix_UB_23      -0.0418998000
_diffrn_orient_matrix_UB_31      0.0749241000
_diffrn_orient_matrix_UB_32      -0.0506631000
_diffrn_orient_matrix_UB_33      -0.0019772000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.661
_diffrn_reflns_theta_min         4.957
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75521
_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.
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    1.296
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.2631
_exptl_crystal_size_mid          0.1445
_exptl_crystal_size_min          0.1012
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0296P)^2^+6.3166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8518
_reflns_number_total             8690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00681h2.cif
_cod_data_source_block           Compound-7
_cod_depositor_comments
'Adding full bibliography for 7049727--7049732.cif.'
_cod_database_code               7049729
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C44 H63 N2 P Se2 Zn'
_reflns_odcompleteness_completeness 99.80
_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), C33(H33), C18(H18), C39(H39), C30(H30), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C34(H34A,H34B), C44(H44A,H44B), C43(H43A,H43B), C36(H36A,
 H36B), C42(H42A,H42B), C35(H35A,H35B), C40(H40A,H40B), C41(H41A,H41B),
 C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C11(H11), C13(H13), C12(H12), C25(H25), C23(H23), C24(H24),
 C6(H6), C7(H7)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'